KR20180028983A - The compressing molding body using complex-fiber and Manufacturing method thereof - Google Patents

Abstract

The present invention relates to a compression molding body and a manufacturing method thereof. More specifically, the present invention relates to a compression molding body compressing a fiber aggregate composed of a bicomponent composite fiber having excellent molding property and shape stability, and a manufacturing method thereof. The fiber aggregate includes the bicomponent composite fiber including a polyester resin and a crystalline polyolefin resin.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a compression-

The present invention relates to a compression-molded body made of a fiber aggregate composed of bicomponent fibers and having excellent shape stability, and a method for producing the same.

Generally, the application of fibrous aggregate such as nonwoven fabric has been used for a variety of purposes such as sanitary, medical, agricultural or industrial use. Particularly in nonwoven fabrics used for industrial purposes, tensile strength is a very important factor. Generally, in order to meet a demand, it is common to use a method of producing a product having a high tensile strength by increasing the weight per unit area. However, since the thickness of the product increases at the same time when the weight is raised, there is a problem that it is difficult to apply the product to a product requiring a small thickness and strength.

Accordingly, a product having a mechanical property similar to or better than that of a plastic product is manufactured and sold by mixing a glass fiber, a carbon fiber, or the like with other fibers, and completing the hologram to complement the deficient mechanical properties of the application product using the fiber aggregate. However, in the case of a product using such a glass fiber, there is a problem that the glass fiber is scattered from the product and contaminated the working environment in the processing step. Glass fiber is known to cause lung cancer. Recently, There is a growing demand for the development of products having properties equal or superior to the physical properties of products using glass fibers.

Korean Patent No. 10-0899613 (Registered on May 20, 2009) Korean Registered Patent No. 10-1357018 (Registered on Apr. 2014)

SUMMARY OF THE INVENTION The object of the present invention is to solve the above-mentioned problems, and an object of the present invention is to provide a fiber aggregate which is excellent in mechanical properties such as tensile strength, flexural strength and flexural modulus, , Sound absorption property, sound diffusing property, water absorption property, water dispersibility and the like, and also to provide a method for producing the same with high commerciality.

In order to solve the above-mentioned problems, the compression-molded article of the present invention comprises a single layer or multiple layers of a fiber aggregate layer obtained by compressing a fiber aggregate comprising a bicomponent fiber including a polyester resin and a crystalline polyolefin resin.

In one preferred embodiment of the present invention, the fibrous assembly may further include a binder fiber in addition to the two-component conjugated fiber.

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

As a preferred embodiment of the present invention, the compression molded article may have an average area density of 600 to 1,500 g / m ² .

In a preferred embodiment of the present invention, the compression molded article may have an average area density uniformity of 2 to 5 CV%.

In one preferred embodiment of the present invention, the compression-molded article of the present invention includes fibers of components other than the fibers constituting the fibrous aggregate layer (first fibrous aggregate layer) in addition to the fibrous aggregate layer (first fibrous aggregate layer) (A second fibrous aggregate layer).

In one preferred embodiment of the present invention, the bicomponent composite fiber comprises a first component resin and a second component resin, wherein the first component resin comprises a polyester resin and the second component resin comprises a crystalline polyolefin resin .

In one preferred embodiment of the present invention, the melting point temperature difference between the first component resin and the second component resin may be 30 ° C to 100 ° C.

In one preferred embodiment of the present invention, the crystalline polyolefin resin may have an enthalpy value of 40 to 120 g / mol, which is necessary for dissolving the crystal in differential thermal analysis (DSC) analysis.

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

In one preferred embodiment of the present invention, the PET resin may include a polymer obtained by polymerizing terephthalic acid and a diol in a molar ratio of 1: 0.95 to 1.20.

In a preferred embodiment of the present invention, the second component resin may include a polyolefin resin containing at least one selected from a polypropylene (PP) resin and a polyethylene (PE) having a melting point of 150 ° C to 170 ° C.

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

In one preferred embodiment of the present invention, the bicomponent conjugate fiber may have a cross-sectional area ratio of 1: 0.5 to 1 for the first component and the second component.

In one preferred embodiment of the present invention, the bicomponent conjugate fiber is a cis-core type fiber, and the sheath contains a crystalline polypropylene (PP) resin having a melting point of 150 ° C to 170 ° C, Terephthalate (PET) resin.

In one preferred embodiment of the present invention, the bicomponent composite fiber has a strength of at least 3.5 g / d, an elongation of at least 55%, an initial modulus of 3.2 g / d or more, a shrinkage of 5.0 to 6.5% And may have a number of 9 to 15 / inch.

In one preferred embodiment of the present invention, the average fiber size of the bicomponent fibers is 4 to 12 d, the average fiber length is 3 to 120 mm, and the number of crimp fibers is 9 to 15 fibers / inch.

In one preferred embodiment of the present invention, the two-component conjugated fiber may have a modified surface, or the surface of the conjugated fiber may have a hydrophilic coating layer and / or a hydrophobic coating layer.

As a preferred embodiment of the present invention, the compression molded article of the present invention may have an average thickness of 2 mm to 5 mm.

As a preferred embodiment of the present invention, the compression molded article of the present invention may have a flexural strength of 5.5 MPa or more and a flexural modulus of 430 MPa or more at a relative humidity of 50% and 23 캜, as measured by ASMT D790.

As a preferred embodiment of the present invention, the compression-molded article of the present invention may have a tensile strength of 18.5 MPa or more at a relative humidity of 50% and 23 캜, as measured by ASMT D638.

Another object of the present invention is to provide a method of producing the above-mentioned compression molded article, which comprises: preparing a fibrous aggregate by using the bicomponent composite fiber, and then laminating the fibrous aggregate into a single layer or multiple layers, A compression molded product can be produced.

In one preferred embodiment of the present invention, the fibrous aggregate may be manufactured by physically entangling a fibrous assembly through a needle punching process.

In one preferred embodiment of the present invention, the fibrous assembly may be prepared by forming a web in a paper making machine by dispersing the bicomponent fibers in water and then performing drying .

As a preferred embodiment of the present invention, the heat treatment may be performed at a temperature of 180 ° C to 220 ° C for 1 minute to 5 minutes.

As a preferred embodiment of the present invention, the compression can be performed by cold compression or hot compression.

In one preferred embodiment of the present invention, the bicomponent composite fiber comprises a first step of preparing a polyester chip and a crystalline polyolefin chip, respectively; A second step in which a first component resin and a second component resin in which a polyester chip and a crystalline polyolefin chip are melted are put into a composite spinneret and mixed and spinned, followed by cooling to produce an unstretched sub-tow; Three steps of stretching the unstretched sub soil and applying crimp; And a fourth step of thermally fixing and cutting the drawn and crimped sub treads.

In one preferred embodiment of the present invention, in the production of the bicomponent composite fiber, the sub tow may be a cis-core type monofilament, a side-by-side type monofilament, a sea-island monofilament, or a split monofilament.

In one preferred embodiment of the present invention, the two-step melting of the bicomponent composite fiber may be performed at a temperature of 270 ° C to 300 ° C and a temperature of 230 ° C to 280 ° C of the crystalline polyolefin chip.

In one preferred embodiment of the present invention, the two-stage composite spinning at the time of producing the bicomponent conjugate fiber can be carried out at a spinning temperature of 260 ° C to 290 ° C and a spinning speed of 400 to 1,300 m / min.

The compression-molded article of the present invention is excellent in physical properties such as tensile strength, flexural strength and flexural modulus, excellent in bonding strength between conjugated fibers and excellent in workability, and has excellent mechanical properties and sound absorption properties, sound dispersibility, It is suitable to be applied to a product which requires the above.

1 (A) and 1 (B) are SEM photographs each showing a section of a compression molded article produced in Production Example 1. FIG.
2A and 2B are SEM photographs each showing a cross-section of the compression molded article produced in Comparative Production Example 1. FIG.
3A and 3B are SEM photographs each showing a section of the compression molded article produced in Comparative Production Example 2. FIG.
4 and 5 are the result of measurement of the morphological stability of Preparation Example 1, Comparative Preparation Example 1 and Comparative Preparation Example 2, which were carried out in Experimental Example 2.

Hereinafter, the compression molded article of the present invention will be described in more detail.

The compression-molded article of the present invention comprises a fibrous aggregate layer (first fibrous aggregate layer) obtained by compressing a fibrous aggregate containing a bicomponent composite fiber comprising a polyester resin and a crystalline polyolefin resin.

In the compression-molded article of the present invention, the fibrous aggregate layer may be composed of a single layer, or may have a multi-layer structure in which a plurality of fibrous aggregate layers are laminated.

In the compression-molded article of the present invention, the fibrous aggregate may contain only the bicomponent conjugate fiber, and may further include binder fibers.

In the present invention, the fibrous aggregate may be a dry-laid nonwoven fabric, a wet-laid nonwoven fabric or an air-laid nonwoven fabric, and various nonwoven fabrics may be applied depending on the use of the compression- .

In addition, the compression-molded article of the present invention is characterized in that, in addition to the above-described fibrous aggregate layer (first fibrous aggregate layer), a fibrous aggregate layer containing fibers of components other than the fibers constituting the fibrous aggregate layer (first fibrous aggregate layer) Fiber aggregate layer) may be further included.

The total thickness of the compression-molded article of the present invention may be an average thickness of 2 mm to 5 mm, preferably an average thickness of 2.5 mm to 4 mm, more preferably 2.5 mm to 3.5 mm, It can be adjusted according to the spec requested by the product.

The compression molded article of the present invention preferably has a flexural strength of 5.5 MPa or more and a flexural modulus of 430 MPa or more when measured at an average thickness of 3 mm (± 0.1 mm) and a relative humidity of 50% and 23 ° C. measured by ASMT D790 A flexural strength of 7.4 to 12 MPa and a flexural modulus of 480 to 700 MPa, more preferably a flexural strength of 9.5 to 11.5 MPa and a flexural modulus of 508 to 620 MPa.

The compression molded product of the present invention has a tensile strength of 18.5 MPa (measured at a relative humidity of 50% and 23 deg. C, a tensile strength of 18.5 MPa Or more, preferably a tensile strength of 20 to 27 MPa, and more preferably 20.2 to 23.5 MPa.

When the average thickness of the press-molded article of the present invention is 3 mm (± 0.1 mm), the average area density may be 600 to 1,500 g / m ² , and preferably the average area density may be 1,000 to 1,400 g / m 2. In addition, the uniformity of the average area density may be 2 to 5 CV%, preferably 3 to 4.8 CV%.

The above-described compression-molded article of the present invention can be produced by preparing a fibrous aggregate by using the bicomponent composite fiber, and then laminating the fibrous aggregate as a single layer or multiple layers, followed by heat treatment and compression.

Here, the fibrous aggregate may be manufactured by performing a general dry nonwoven fabric manufacturing process in the related art. In one preferred embodiment, the fibrous aggregate is produced by physically entangling a bicomponent conjugate fiber through a needle punching process .

In addition, the fibrous aggregate can be produced by performing a general wet nonwoven fabric manufacturing process in the related art. In one preferred embodiment, a dispersion in which the bicomponent conjugate fiber is dispersed in water is dispersed in a paper web And then performing the drying step.

In the method for manufacturing a compression molded article of the present invention, the heat treatment may be performed at a temperature of 180 ° C to 220 ° C for 1 minute to 5 minutes, preferably at a temperature of 190 ° C to 210 ° C for 1 minute to 3 minutes.

In the method of manufacturing a compression molded article of the present invention, the compression may be performed by cold compression or thermal compression.

Hereinafter, the bicomponent composite fiber constituting the fiber aggregate layer constituting the compression-molded article of the present invention will be described.

[Binary conjugate fiber]

In the present invention, the bicomponent conjugate fiber is a bicomponent conjugate fiber comprising a first component resin and a second component resin, wherein the sheath-core type fiber, the side-by-side may be a sea-island-type fiber, a sea-islands-type fiber or a segmented-pie-type fiber, and preferably a cis-core type fiber or a side-by-side type fiber.

The first component resin is related to the shape stability of a fiber aggregate such as a nonwoven fabric and a compression molded product produced using the same, and it is preferable to use a resin having an excellent modulus. Further, it is preferable to adopt a material suitable for securing the form stability and moldability of the fiber aggregate and / or the compression-molded body by ensuring the adhesiveness between the composite fibers of the second component resin.

In the bicomponent bicomponent fiber of the present invention, the difference in melting point temperature of the first component resin and the second component resin may be 30 ° C. to 100 ° C., preferably 40 ° C. to 90 ° C. At this time, If the temperature is lower than 30 ° C, the fibrous aggregate must be produced under a proper temperature atmosphere so that the second component resin is appropriately melted so as to be bonded between the conjugate fibers due to the second component resin in the production of the fibrous aggregate using the conjugate fiber. And the first component resin is disadvantageous because the temperature difference between the melting point of the second component resin is small, there is a problem that the mechanical properties of the fiber aggregate and the compression molded product using the fiber aggregate are reduced and the workability and formability are poor. , The temperature difference between resins becomes unnecessarily too large, and the compatibility between the resins of the first and second components is lowered, so that it is difficult to produce the bicomponent composite fiber I could be.

(PET) resin, a polybutylene terephthalene (PBT) resin, a polytrimethylene terephthalate (PTT) resin, and a polyethylene terephthalate Phthalate (PEN) resin, and may preferably include at least one selected from a PET resin, a PBT resin and a PEN resin, more preferably a PET resin.

The polyester resin preferably has an intrinsic viscosity of 0.50 to 1.00 dl / g and a melting point of 200 ° C or higher, preferably an intrinsic viscosity of 0.55 to 0.90 dl / g and a melting point of 230 ° C to 280 ° C, more preferably an intrinsic viscosity of 0.60 To 0.75 dl / g and a melting point of 240 ° C to 265 ° C. At this time, if the intrinsic viscosity of the polyester resin is less than 0.50 dl / g, the strength of the composite fiber may be lowered. If the intrinsic viscosity exceeds 1.00 dl / g, there may be a problem that spinning and drawing workability is inferior . If the melting point of the PET resin is less than 200 占 폚, the difference in melting point between the second component resin and the second component resin may become too small, resulting in a problem of poor processability and moldability during production of an application product using the conjugate fiber. It is better to use resin.

When the polyester resin is a PET resin, it is possible to use a general PET resin used in the art, preferably a polymer obtained by polymerizing terephthalic acid and a diol in a molar ratio of 1: 0.95 to 1.20 Can be used.

Next, the second component resin may include a polyolefin resin.

As the crystalline polyolefin resin, at least one selected from a polypropylene resin and a polyethylene resin can be used, and a polypropylene resin can be preferably used.

The crystalline polyolefin resin preferably has an enthalpy value of 20 to 30 J / g, preferably 22 to 28 J / g, in terms of an enthalpy value necessary for dissolving the crystal in DSC (differential thermal analysis) .

The crystalline polyolefin resin preferably has a melting point of 150 to 170 캜, preferably 155 to 170 캜, more preferably 160 to 170 캜, wherein the crystalline polyolefin resin has a melting point of less than 150 캜 The difference in melting point temperature between the first component resin and the polyester resin becomes too large to lower the radioactivity for the production of the bicomponent conjugate fiber and the compatibility of the first component and the second component in the resin decreases to produce the bicomponent conjugate fiber There may be a difficult problem. If the melting point exceeds 170 DEG C, there may be a problem that the difference in melting point between the first and second component resins becomes small, resulting in deteriorated workability.

The two-component bicomponent fiber may be a bicomponent fiber composed of bicomponent fibers. The fibers may have a cross-sectional area ratio of 1: 0.5 to 1, preferably a cross-sectional area ratio of 1: 0.7 to 1, for the first component and the second component. If the ratio of the second component cross-sectional area is less than 0.5, there may be a problem that the bonding strength between the conjugate fibers is lowered. If the ratio of the second component cross-sectional area exceeds 1, the area of the first component is relatively decreased and the strength of the conjugate fiber is weakened. There may be a problem in that the modulus of the product produced by the use decreases.

The composite fiber according to the present invention is a cis-core type conjugate fiber, wherein the sheath contains a crystalline polypropylene (PP) resin having a melting point of 150 ° C to 170 ° C, The core may comprise a polyethylene terephthalate (PET) resin having a melting point of at least 200 ° C.

The average fiber size of the bicomponent composite fibers is 4-12 d, the average fiber length is 3-120 mm, the number of crimp is 9-15 fibers / inch, the average fineness is 5-10 d, The average fiber length may be 6 to 100 mm, the crimp number may be 10 to 14, more preferably the average fineness is 5 to 9 de, the average fiber length may be 20 to 100 mm, and the crimp number may be 10 to 14. At this time, if the average fineness of the conjugate fiber is less than 4 de, there may be a problem that the tensile strength of the fiber aggregate and / or the compression molded article is lowered, and when the deodorization strength exceeds 12 de, the modulus of the fiber aggregate and / Can be. The fiber length of the composite fiber can be changed by changing the fiber length of the composite fiber according to the product to be manufactured using the composite fiber. If the number of crimps is less than 9 / inch, the elasticity and bulging property of the composite fibers may deteriorate. If the number of crimps exceeds 15 / inch, there may be a problem of increasing the occurrence of neps in the carding process have.

The bicomponent conjugate fiber may modify the surface of the fiber to impart functionality, or the hydrophilic coating layer and / or the hydrophobic coating layer may be formed on the surface of the conjugate fiber.

The bicomponent composite fibers used in the present invention may have a strength of at least 3.5 g / d, an elongation of at least 55%, an initial modulus of at least 3.2 g / d, a shrinkage of 5.0 to 6.5% and a crimp number of 9 to 15 / And preferably has a strength of 3.70 to 4.10 g / d, an elongation of 57 to 62%, an initial modulus of 3.2 to 3.8 g / d, a shrinkage of 5.4 to 6.2% and a crimp number of 10 to 14 / inch.

The two-component bicomponent fiber may include a first step of preparing a polyester chip and a crystalline polyolefin chip, respectively; A second step in which a first component resin and a second component resin in which a polyester chip and a crystalline polyolefin chip are melted are put into a composite spinneret and mixed and spinned, followed by cooling to produce an unstretched sub-tow; Three steps of stretching the unstretched sub soil and applying crimp; And a fourth step of thermally fixing and cutting the drawn and crimped sub treads.

The characteristics, kinds, and the like of the polyester chip in the first step are the same as those of the first component resin described above, and the characteristics, kinds and the like of the crystalline polyolefin chip are the same as those of the second component resin described above, And the second component resin is a chip.

The two-step melting can be performed at a temperature of 270 ° C to 300 ° C, and a crystalline polyolefin chip can be performed at a temperature of 230 ° C to 280 ° C.

The composite spinning in two stages can be carried out under conditions of a spinning temperature of 260 to 290 DEG C and a spinning speed of 400 to 1,300 m / min, preferably 265 to 285 DEG C and a winding speed of 500 to 1,200 m / min. At this time, if the spinning temperature is less than 260 캜, there may be a problem that the pack internal pressure rise and spinning workability are lowered, and if the spinning temperature exceeds 290 캜, there may be a problem that the physical properties of the composite fiber are deteriorated. If the coiling speed is less than 500 m / min, the elongation may increase and the properties of the composite fiber and / or the application product using the composite fiber may be deteriorated. If the coiling speed exceeds 1,300 m / min, There is a problem that the shape to be laminated on the can is uneven and the drawing workability is lowered.

The two-stage sub tou can be a sheath-core type monofilament, a side-by-side type monofilament, a sea-island monofilament, or a split monofilament.

The three-step stretching can be performed by a general method used in the art. Preferably, the unstretched sub-tow is stretched at a temperature of 70 to 100 DEG C at a stretching rate of 2.5 to 5 times, preferably 3.0 to 4.5 times can do. If the stretching ratio is less than 2.5 times, elongation increases, and the physical properties of the applied product using the conjugate fiber may be decreased. When the stretching ratio exceeds 5.0 times, there may be a problem that yarns are formed. It is good.

The three-step crimping can be performed by a conventional crimping method as used in the art. For example, a crimp box capable of passing the drawn sub toupe at 3,000 to 8,000 de / The crimping can be performed through the process.

Further, it is possible to additionally perform a step of performing a suit heat treatment process on the sub-tow drawn before crimping to improve the stability of the sub-tow. For example, a plurality of hot drums may be used to heat the surface of the hot drum For 5 seconds to 30 seconds to heat treatment to increase the degree of crystallization of the sub-tow, thereby improving the shrinkage and the modulus of elasticity.

The four-stage heat setting can be carried out through a general heat fixing method used in the art. As a preferable example, the stretched and crimped sub tow is put into an oven and then heated at a temperature of 140 ° C to 180 ° C, Can be carried out at a temperature of 140 ° C to 170 ° C for 10 to 20 minutes. If the heat setting temperature is lower than 140 ° C, there may be a problem that the shrinkage ratio of the final composite fiber produced increases. If the temperature is higher than 180 ° C, the dispersibility of the composite fiber deteriorates to decrease the composite fiber density of the fiber aggregate. It is preferable to perform heat fixing under the above temperature range.

The four-step cutting is a step of cutting the sub-tow which is heat-fixed so that the composite fiber has an appropriate fiber length according to the product to be used, and can be performed by a general cutting method used in the art, It is preferable that the cutting is performed within the range of 3 mm to 120 mm in average fiber length of the composite fibers.

As described above, the composite fiber of the present invention can be produced by the above manufacturing method as long as the average fineness is 4 to 12 de, the average fiber length is 3 to 120 mm, and the number of crimps is 9 to 15 fibers / inch. have.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples should not be construed as limiting the scope of the present invention, and should be construed to facilitate understanding of the present invention.

[ Example ]

Example  One : Cis - Core type  Manufacture of composite fibers

A PET chip in which a polyethylene terephthalate (PET) resin having an intrinsic viscosity of 0.65 dl / g and a melting point of 252 ° C was chipped was prepared.

Further, a PP chip obtained by chipping a polypropylene (PP) resin having an enthalpy value of 94 J / g and a melting point of 165 DEG C necessary for dissolving the crystal was prepared in DSC (differential thermal analysis) analysis.

Next, the PET chips were melted at 290 ° C and the PP chips were melted at 260 ° C, and then they were put in a composite spinneret and spun, and then cooled to prepare cis-core type unoriented-subtowels.

At this time, the composite spinning was carried out at a spinning temperature of 275 ° C and a coiling speed of 950 m / min, and the composite spinning was carried out through the drawing process and loaded on the can.

Next, the unstretched-subtow was stretched 3.2 times at 85 캜, and then subjected to a suit heat treatment at 150 캜 for 10 seconds.

Next, the drawn sub toe was crimped using a sparging box.

Next, the stretched and crimped sub treads were put in an oven and then heat-set at 165 ° C for 15 minutes to prepare cis-core type conjugated fibers having an average fineness of 7 de, an average fiber length of 51 mm and a number of crimps of 11 per inch . At this time, the cross sectional area ratio between sheath and core was 1: 1, the sheath was made of PP resin, and the core was made of PET resin.

Example  2 ~ Example  12 and Comparative Example  1 to 10

The same procedure as in Example 1 was carried out except that the PET chip as the core component, the PP chip as the sheath component, the average fineness, the average fiber length, the crimp number, and the cross- Cis-core type conjugate fibers were respectively prepared and Examples 2 to 12 and Comparative Examples 1 to 10 were carried out.

division Intrinsic viscosity
(dl / g) Melting point Fusing DSC The average fineness (de),
Average fiber length (mm) /
Crimp number (in / inch) Sys: Core
Sectional area ratio Example 1 core PET 0.65 252 DEG C 87 ℃ * 7de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Example 2 core PET 0.65 252 DEG C 82 ° C * 7de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 170 ℃ 90 J / g Example 3 core PET 0.65 242 ° C 87 ℃ * 7de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 155 ℃ 95 J / g Example 4 core PET 0.55 241 DEG C 78 ℃ * 7de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Example 5 core PET 0.90 260 ℃ 95 ℃ * 7de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Example 6 core PET 0.65 252 DEG C 87 ℃ * 7de,
51 mm,
11 pieces / inch 1: 0.7 Cis PP * 165 ° C 94 J / g Example 7 core PET 0.65 252 DEG C 87 ℃ * 10deg,
51 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Example 8 core PET 0.65 252 DEG C 87 ℃ * 5de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Example 9 core PET 0.65 252 DEG C 87 ℃ * 7de,
95 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Example 10 core PET 0.65 252 DEG C 87 ℃ * 7de,
25 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Example 11 core PET 0.65 252 DEG C 87 ℃ * 7de,
51 mm,
14 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Example 12 core PET 0.65 252 DEG C 87 ℃ * 7de,
51 mm,
9 / inch 1: 1 Cis PP * 165 ° C 94 J / g

division Intrinsic viscosity
(dl / g) Melting point Fusing DSC The average fineness (de),
Average fiber length (mm) /
Crimp number (in / inch) Sys: Core
Sectional area ratio Comparative Example 1 core PET 0.65 252 DEG C 82 ° C * 7de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 176 ° C 89 J / g Comparative Example 2 core PET 0.65 242 ° C 87 ℃ * 7de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 148 DEG C 97 J / g Comparative Example 3 core PET 0.46 240 ℃ 75 ℃ * 7de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Comparative Example 4 core PET 1.05 262 DEG C 97 ℃ * 7de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Comparative Example 5 core PET 0.65 252 DEG C 87 ℃ * 7de,
51 mm,
11 pieces / inch 1: 0.45 Cis PP * 165 ° C 94 J / g Comparative Example 6 core PET 0.65 252 DEG C 87 ℃ * 7de,
51 mm,
11 pieces / inch 1: 1.14 Cis PP * 165 ° C 94 J / g Comparative Example 7 core PET 0.65 252 DEG C 87 ℃ * 12.6de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Comparative Example 8 core PET 0.65 252 DEG C 87 ℃ * 3.7de,
51 mm,
11 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Comparative Example 9 core PET 0.65 252 DEG C 87 ℃ * 7de,
51 mm,
16 pieces / inch 1: 1 Cis PP * 165 ° C 94 J / g Comparative Example 10 core PET 0.65 252 DEG C 87 ℃ * 7de,
51 mm,
8 / inch 1: 1 Cis PP * 165 ° C 94 J / g

Experimental Example  1: Measurement of physical properties of composite fiber

The strength, elongation, initial elastic modulus and shrinkage of the composite fiber were measured according to the following methods, and the results are shown in Table 3 below.

1) How to measure tenacity and elongation

Steel fiber and elongation of the fiber were measured using an automatic tensile tester (Textechno) at a speed of 50 cm / m and a grip distance of 50 cm. The strength and elongation are determined by dividing the load (d) by the denier when the fiber is stretched until it is cut by a constant force, and the value (%) of the initial length as a percentage of the elongated length Respectively.

2) initial modulus, Contraction ratio  How to measure

The initial modulus of elasticity was measured by a USTER TESTER and the shrinkage ratio was measured according to the following equation (1) after changing the length of the composite fiber before and after the heat treatment at 180 for 20 minutes.

[Equation 1]

Shrinkage (%) = (C-D) / C 100%

In the formula (1), C is the average length of the fibers before the heat treatment, and D is the average length of the fibers after the heat treatment.

division burglar
(%) Shindo
(%) Initial modulus
(g / de) Contraction ratio
(%) Crimp number
(Dogs / inch) Example 1 3.89 59.2 3.5 5.7 10.8 Example 2 3.92 57.3 3.5 5.8 10.9 Example 3 3.84 59.1 3.6 5.8 10.9 Example 4 3.71 57.4 3.5 5.7 11.2 Example 5 4.08 58.1 3.3 5.7 10.8 Example 6 3.82 58.8 3.4 5.7 11.0 Example 7 3.85 59.9 3.7 5.6 10.9 Example 8 3.92 58.6 3.6 5.8 11.0 Example 9 3.88 59.5 3.6 5.6 11.0 Example 10 3.91 58.3 3.5 6.0 10.8 Example 11 3.82 61.7 3.6 5.7 13.6 Example 12 3.94 57.8 3.4 5.5 10.1 Comparative Example 1 3.77 57.1 3.0 5.7 11.1 Comparative Example 2 No spinning Comparative Example 3 3.45 55.3 3.4 5.8 10.7 Comparative Example 4 4.18 54.2 3.4 5.6 10.9 Comparative Example 5 3.14 48.5 3.6 5.6 11.1 Comparative Example 6 3.58 65.2 3.7 5.4 11.0 Comparative Example 7 No spinning Comparative Example 8 No spinning Comparative Example 9 3.72 58.3 3.5 7.5 16.3 Comparative Example 10 3.82 60.7 3.6 5.1 7.8

The results of physical properties of the composite fibers shown in Table 3 were as follows: Examples 1 to 12 had strength of 3.71 to 4.08 g / d, elongation of 57.3 to 61.7%, initial modulus of 3.3 to 3.6 g / d, shrinkage of 5.5 to 6.0% And a number of crimps of 9.3 to 13.5 / inch.

On the contrary, Comparative Example 1 using a resin having a sheath component melting point exceeding 170 ° C had a low initial elastic modulus of less than 3.2 g / d, and in Comparative Example 2 having a sheath component melting point of less than 150 ° C, It was impossible to measure the physical properties of the composite fiber.

In addition, in Comparative Example 3 in which PET having an intrinsic viscosity of 1.0 dl / g or more was incorporated as a core component, the strength and elongation were lower than those of Examples.

In Comparative Example 5 in which the cross-sectional area ratio of the sheath and core of the composite fiber was 1: 0.45, which was less than 1: 0.5, there was a problem that the elongation was extremely poor.

In addition, in Comparative Example 7 in which the average fiber size of the composite fibers exceeded 12 de and in Comparative Example 8 in which the average fiber size was less than 4 de, the spinning was practically impossible.

 In the case of Comparative Example 9 in which the number of crimps exceeded 16 / inch, there was a problem that the number of crimps was excessively formed exceeding 15 crimps / inch, and in Comparative Example 10 in which the crimp number was less than 9 crimps / inch, .

Manufacturing example  One : Of the compression molded article  Produce

Carded using only the composite fibers prepared in Example 1 to produce a needle punching nonwoven fabric having a thickness of 10 mm.

Next, the non-woven fabric was heat-treated at 200 ° C for 90 seconds, and then cold-pressed to produce a compression molded product (average thickness of 3 mm).

The average area density of the produced compression molded product was 1,230 g / m ² , and the average area density uniformity was 3 CV%.

Manufacturing example  2 : Of the compression molded article  Produce

PET having a density of 7 denier, a fiber length of 51 mm and an intrinsic viscosity of 0.65 dl / g was mixed in an amount of 50% by weight, and then carded to form a 10 mm thick needle punching nonwoven fabric Respectively.

Next, a heat treatment process and cold compression were carried out in the same manner as in Production Example 1 to prepare a compression molded product (average thickness 3 mm).

The average compactness of the compacts thus prepared was 1,250 g / m ² , and the average area density was 4.6 CV%.

Manufacturing example  3: Of the compression molded article  Produce

7-denier and fiber length 51 mm short fibers of 70% by weight of the composite fiber prepared in Example 1 and having an intrinsic viscosity of 0.65 dl / g were mixed at 30% by weight, and carded to form a 10 mm thick needle punching. Nonwoven fabric was produced.

Next, a heat treatment process and cold compression were carried out in the same manner as in Production Example 1 to prepare a compression molded product (average thickness 3 mm).

The average compactness of the produced compacted article was 1,210 g / m < ² > and the uniformity of the average area density was 3.8% CV.

Manufacturing example  4 ~ Manufacturing example  14: Of the compression molded article  Produce

A 10 mm thick needle punching nonwoven fabric was produced by the same method as in Example 1 except that the composite fibers of Examples 2 to 12 were used instead of the composite fibers of Example 1 by carding.

Next, the non-woven fabric was heat-treated at 200 ° C for 90 seconds, and then cold-pressed to obtain a compression molded product (average thickness of 3 mm), and Production Examples 4 to 14 were carried out respectively (see Table 4 below).

Comparative Manufacturing Example  One

9 denier, 60 wt% of mono type polypropylene fibers having a fiber length of 70 mm and 40 wt% of glass fibers, and then carded to produce a 10 mm thick needle punching nonwoven fabric.

Next, a heat treatment process and cold compression were carried out in the same manner as in Production Example 1 to prepare a compression molded product (average thickness 3 mm).

Comparative Manufacturing Example  2

50% by weight of PET binder fibers having a softening point of 4 탆, a fiber length of 51 mm, and 50% by weight of PET short fibers having a density of 7 denier, a fiber length of 51 mm and an intrinsic viscosity of 0.65 dl / g were mixed, Thereby producing a needle punching nonwoven fabric.

Next, a heat treatment process and cold compression were carried out in the same manner as in Production Example 1 to prepare a compression molded product (average thickness 3 mm).

Comparative Manufacturing Example  3 to 9: Of the compression molded article  Produce

A 10 mm thick needle punching nonwoven fabric was produced by the same method as in Example 1 except that the composite fibers of Comparative Examples 1 to 10 were used instead of the composite fibers of Example 1 by carding.

Next, the non-woven fabric was heat-treated at 200 ° C for 90 seconds and then cold-pressed to obtain a compression molded product (average thickness of 3 mm), and Comparative Production Examples 3 to 9 were carried out respectively (see Table 4 below) .

division Conjugated fiber Mixed fiber Mixed fiber and PET fiber mixed amount Production Example 1 Example 1 * 100 wt% Production Example 2 Example 1 7 denier, a fiber length of 51 mm, an intrinsic viscosity of 0.65 dl / g, Composite fiber 50 wt%
+
50% by weight of PET short fibers Production Example 3 Example 1 7 denier, a fiber length of 51 mm, an intrinsic viscosity of 0.65 dl / g, Composite fiber 70 wt%
+
PET staple fibers 30 wt% Production Example 4 Example 2 * 100 wt% Production Example 5 Example 3 * 100 wt% Production Example 6 Example 4 * 100 wt% Production Example 7 Example 5 * 100 wt% Production Example 8 Example 6 * 100 wt% Production Example 9 Example 7 * 100 wt% Production Example 10 Example 8 * 100 wt% Production Example 11 Example 9 * 100 wt% Production Example 12 Example 10 * 100 wt% Production Example 13 Example 11 * 100 wt% Production Example 14 Example 12 * 100 wt% Comparative Preparation Example 1 9 denier, 70 mm fiber length Mono type polypropylene (PP) fiber Glass fiber PP fiber 60 wt%
+
40% by weight of glass fiber Comparative Production Example 2 4 denier, PET fiber having a fiber length of 51 mm and a softening point of 110 ° C 7 denier, a fiber length of 51 mm, an intrinsic viscosity of 0.65 dl / g, PET binder fiber 50 wt%
+
50% by weight of PET short fibers Comparative Production Example 3 Comparative Example 1 * 100 wt% Comparative Production Example 4 Comparative Example 3 * 100 wt% Comparative Preparation Example 5 Comparative Example 4 * 100 wt% Comparative Preparation Example 6 Comparative Example 5 * 100 wt% Comparative Preparation Example 7 Comparative Example 6 * 100 wt% Comparative Preparation Example 8 Comparative Example 9 * 100 wt% Comparative Preparation Example 9 Comparative Example 10 * 100 wt%

Experimental Example  One : Of the compression molded article SEM  Measure

SEM photographs of the cut surfaces of the compression molded articles produced in Production Example 1, Production Example 2 and Production Example 3 are shown in Fig. 1 to Fig. 3, respectively.

The SEM measurement photographs of FIG. 1 show that, in the case of the compression molded article of the present invention, the fibers are formed in a dense fashion, whereas in the case of Production Examples 2 and 3, as shown in FIGS. 2 and 3, Respectively.

Experimental Example  2 : Of the compression molded article  Shape stability measurement

1) Morphological stability according to temperature

The compression molded product prepared in Preparation Example 1, Comparative Production Example 1 and Comparative Production Example 2 was put into a hot-air drier and the shape was changed after aging for 1 hour under a load of 80 g. The results are shown in FIG.

4, the compression molded product of Production Example 1 showed excellent shape stability even at 100 ° C and 110 ° C, whereas Comparative Production Examples 1 and 2 had a problem of poor shape stability at 100 ° C .

2) Measurement of shape stability after aging of heat-resistant environment

The molded articles prepared in Preparation Example 1, Comparative Preparation Example 1 and Comparative Preparation Example 2 were allowed to stand in a heat-resistant environment, and then their external force was removed and then their shape stability after 72 hours at 80 ° C was measured. Respectively.

5, in the case of Production Example 1, there was almost no change in shape, but in Comparative Production Example 1, it was greatly bent, and in Comparative Production Example 2, the end portion was slightly curled while being curled.

It was confirmed that the molded article prepared from the conjugate fiber of the present invention had excellent dimensional stability through measurement of shape stability.

Experimental Example  3: Of the compression molded article  The tensile strength, Modulus  Measure

The tensile strength, flexural strength and flexural modulus of the compression-molded products produced in Production Examples 1 to 14 and Comparative Production Examples 1 to 12 were measured, and the results are shown in Table 5 below.

At this time, the tensile strength was measured according to ASTM D 638, and the modulus of bending strength and flexural modulus were measured according to ASTM D 790.

In addition, the uniformity means a standard deviation value at the time of measuring the average area density.

division The tensile strength
(Mpa) Flexural strength
(Mpa) Flexural modulus
(Mpa) Average area density
(g / m ² ) Average area density
Homogeneity of
(CV%) Production Example 1 21.3 9.7 542 1,230 3.0 Production Example 2 18.5 5.7 436 1,250 4.6 Production Example 3 20.6 7.4 480 1,210 3.8 Production Example 4 20.8 9.6 537 1,230 4.1 Production Example 5 21.5 9.4 518 1,190 4.3 Production Example 6 20.3 9.2 495 1,200 3.5 Production Example 7 20.4 10.7 583 1,210 4.3 Production Example 8 20.7 9.1 522 1,200 5.1 Production Example 9 20.7 10.1 531 1,190 3.5 Production Example 10 21.1 9.5 508 1,220 3.8 Production Example 11 23.1 9.3 511 1,220 4.4 Production Example 12 20.4 9.5 502 1,230 4.1 Production Example 13 20.4 10.0 545 1,210 4.2 Production Example 14 21.2 9.2 551 1,220 4.2 Comparative Preparation Example 1 9.5 3.2 316 1,200 3.5 Comparative Production Example 2 9.0 2.8 125 1,190 3.8 Comparative Production Example 3 20.1 8.9 471 1,200 4.4 Comparative Production Example 4 20.4 7.7 448 1,230 4.3 Comparative Preparation Example 5 18.8 9.8 490 1,200 4.1 Comparative Preparation Example 6 19.7 5.9 411 1,210 4.0 Comparative Preparation Example 7 19.4 7.4 420 1,220 4.0 Comparative Preparation Example 8 18.6 9.4 483 1,190 3.8 Comparative Preparation Example 9 18.9 9.5 490 1,180 3.9

As shown in Table 5, it was confirmed that the compression molded products of Production Examples 1 to 14 were superior in overall tensile strength and modulus to those of Comparative Production Examples 1 to 2. In Production Example 1 using the fibers for compression molded product alone, The results are shown in Table 1. The results are shown in Table 1. The results are shown in Table 1.

In Comparative Production Example 3, there was a problem that the bending strength was somewhat lowered and the workability was poor. In Comparative Production Example 4, flexural modulus was not good.

In Comparative Production Example 5, the bending strength was excellent but the tensile strength was somewhat lower. In Comparative Production Example 6 and Comparative Production Example 7, the bending strength and flexural modulus were too low.

Also, in Comparative Production Example 8, there was a problem that the number of crimp of the used composite fiber was high and a nep occurred, and in Comparative Production Example 9, the number of crimp of the composite fiber used was too low and the flexural modulus was low .

Through the above Examples and Experimental Examples, it was confirmed that the conjugate fiber of the present invention has excellent mechanical properties and sound absorption / sound dispersibility and water absorption / water dispersibility. It is expected that the composite fiber of the present invention can be made into a fibrous aggregate such as a nonwoven fabric or the fibrous aggregate can be compressed to provide various application products. Specific examples thereof include architectural interior / exterior materials / civil engineering materials / A sanitary material such as a diaper, a sanitary napkin, and a mask, a filter such as an air filter or a liquid filter, and the like.

Claims (15)

The fibrous aggregate layer in which the fibrous aggregate is compressed includes a single layer or multiple layers,
Wherein the fiber aggregate comprises a bicomponent composite fiber comprising a polyester resin and a crystalline polyolefin resin.
The compression molded article according to claim 1, wherein the fibrous aggregate further comprises binder fibers.
The compression-molded body according to claim 1, wherein the fibrous aggregate is a dry-laid nonwoven fabric, a wet-laid nonwoven fabric, or an air-laid nonwoven fabric.
The compression molded article according to claim 1, wherein the compression molded article has an average area density of 600 to 1,500 g / m ² .
The compression-molded body according to claim 4, wherein the uniformity of the average area density is 2 to 5 CV%.
The bicomponent fiber of claim 1, wherein the bicomponent composite fiber comprises a sheath-core type fiber, a side-by-side type fiber, a sea- segmented-pie-type fibers.
2. The polyester resin composition according to claim 1, wherein the polyester resin has an intrinsic viscosity of 0.50 to 1.00 dl / g and a melting point of 200 ° C or more, and the polyester resin is selected from the group consisting of polyethylene terephthalate (PET) resin, polybutylene terephthalene (PBT) (PTT) resin, and polyethylene naphthalate (PEN) resin.
Wherein the crystalline polyolefin resin comprises at least one selected from a polypropylene (PP) resin and a polyethylene (PE) having a melting point of 120 ° C to 170 ° C.
The composite fiber according to claim 1, wherein the bicomponent composite fiber is a cis-core type fiber, the sheath is a crystalline polyolefin resin, the core comprises a polyester resin,
Characterized in that the sheath-core type fiber has an average fineness of 4 to 12 de, an average fiber length of 3 to 120 mm, and a crimp number of 9 to 15 / inch.
The compression molded article according to claim 1, wherein the compression molded article has an average thickness of 2 mm to 5 mm.
The compression molded article according to claim 1, wherein the flexural strength is 5.5 MPa or more and the flexural modulus is 430 MPa or more at a relative humidity of 50% and 23 캜 measured by ASMT D790.
The compression molded article according to claim 1, wherein the tensile strength is 18.5 MPa or more when measured at ASMT D638 at relative humidity of 50% and 23 캜.
A method for producing a nonwoven fabric composite by using the bicomponent composite fiber and then laminating the fibrous aggregate as a single layer or multiple layers, followed by heat treatment, followed by compression.
[14] The method of claim 12, wherein the fibrous assembly is manufactured by physically entangling the fibrous assembly through a needle punching process.
[12] The method according to claim 12, wherein the fibrous aggregate is produced by forming a web in a paper machine using a dispersion in which the bicomponent fibers are dispersed in water, followed by drying. ≪ / RTI >
13. The bicomponent fiber according to claim 12, wherein the bicomponent composite fiber comprises a polyester resin and a crystalline polyolefin resin,
Wherein the bicomponent composite fiber is a cis-core type fiber, a side-by-side type fiber, a sea-island type fiber or a split type fiber.

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