KR101959679B1 - polyester composition for thermally adhesive fiber and thermally adhesive composite fiber containing the same - Google Patents

Abstract

The present invention relates to a polyester composition for thermally adhesive fibers and thermally adhesive composite fibers comprising the same. More specifically, the present invention relates to: the polyester composition for thermally adhesive fibers which is flexible when adhering the same, can exhibit soft feel, and has a low density; and thermally adhesive composite fibers having excellent color when dyeing the same under low temperature and low pressure conditions by comprising the polyester composition for thermally adhesive fibers according to the present invention.

Description

TECHNICAL FIELD [0001] The present invention relates to a polyester composition for thermally adhesive fibers and a thermally adhesive composite fiber comprising the thermally adhesive fiber,

The present invention relates to a polyester composition for heat-bondable fibers and a thermally adhesive composite fiber comprising the same, and more particularly to a polyester composition for thermally adhesive fibers, which is flexible, An ester composition and a polyester composition for a heat-bondable fiber according to the present invention and having excellent color yield in dyeing under low-temperature and low-pressure conditions.

Generally, polyester is a generic term of a polymer compound having an ester bond (-COO) in a molecule, such as an unsaturated polyester resin, an alkyd resin, and a thermoplastic polyester resin typified by polyethylene terephthalate (PET).

Such a polyester fiber has a high strength, a chemical resistance, a melting point in the range of 250 to 255 占 폚, excellent heat resistance, and elasticity against elongation flexure, Varies.

However, the above-mentioned polyester has a relatively high melting point. Generally, when the fiber structure is cured, an adhesive containing a formalin (aqueous formaldehyde solution) or an organic solvent, a hard resin (phenol resin, melanin resin, urea resin) is used. The adhesive containing such an organic solvent does not penetrate into the inside of the fabric, and the adhesiveness is low, and the feeling when finished is rough. In addition, most of the substances are highly volatile and harmful to human body, and there are environmental problems such as toxic gas discharge.

In addition, the conventional polyester-based composite fiber composed of the sheath portion and the core portion has a low melting point polyester in the sheath portion. However, since the flexibility is very low and the feel is rough during the bonding, There is a problem that a high-temperature and high-pressure environment is required in dyeing the fiber.

Korean Patent Publication No. 10-2007-0034648

Disclosure of the Invention The present invention has been made in view of the above-mentioned problems, and it is an object of the present invention to provide a polyester composition for thermally adhesive fibers which is flexible and exhibits soft touch and has low density, and a polyester composition for thermally adhesive fibers Which is excellent in color yield in dyeing under low temperature and low pressure conditions.

Another object of the present invention is to provide an interior yarn comprising the thermosetting conjugate fiber according to the present invention.

In order to solve the above-mentioned problems, the present invention provides a process for producing a polyester resin composition, which comprises reacting an acid component containing terephthalic acid and a diol component comprising ethylene glycol and 2-methyl-1,3-propanediol in the presence of an esterified compound and a polyalkylene glycol, A thermoplastic polyester resin, and a thermoplastic resin.

According to one embodiment of the present invention, the diol component may be substantially free of diethylene glycol.

According to an embodiment of the present invention, the polyalkylene glycol may be contained in an amount of 1 to 10% by weight based on the weight of the esterified compound.

According to an embodiment of the present invention, the polyalkylene glycol may be polyethylene glycol.

According to an embodiment of the present invention, the polyethylene glycol may have a weight average molecular weight of 400 to 12,000.

According to an embodiment of the present invention, the weight average molecular weight may be 400 to 6000.

According to an embodiment of the present invention, the esterification compound may include the acid component and the diol component in a molar ratio of 1: 1 to 1: 2.

According to an embodiment of the present invention, the 2-methyl-1,3-propanediol may be contained in an amount of 25 to 40 mol% of the diol component.

According to an embodiment of the present invention, the 2-methyl-1,3-propanediol may be contained in an amount of 29 to 40 mol% of the diol component.

According to another embodiment of the present invention, there is provided a polyester composition for thermally adhesive fibers, wherein the acid component further comprises isophthalic acid in an amount of 1 to 15 mol% of the acid component.

According to an embodiment of the present invention, the copolyester includes an acid component of terephthalic acid, a diol component composed of 60 to 71 mol% of ethylene glycol and 29 to 40 mol% of 2-methyl-1,3-propanediol The esterified compound reacted at a molar ratio of 1: 1 to 1: 2 and the polyethylene glycol having a weight average molecular weight of 400 to 6000, which is contained in an amount of 1 to 10% by weight based on the weight of the esterified compound, may be polycondensed .

The present invention also provides a thermosetting conjugate fiber comprising a core portion comprising a polyester component and a sheath portion including a polyester composition for a thermally adhesive fiber according to the present invention surrounding the core portion.

According to an embodiment of the present invention, the composite fibers are mixed with polyethylene terephthalate staple fibers at a weight ratio of 1: 1 and then heat-treated at 140 ° C to obtain fibers having a width, a length, and a thickness of 100, 20, When it is implemented as a specimen, it can have an adhesive strength of 100 N or more when measuring the bonding strength by UTM (universal testing machine) according to KS M ISO 36 method.

According to an embodiment of the present invention, the conjugate fiber is mixed with a salt solution containing 2% by weight of dyes (C.I. Basic Blue 54) based on the weight of the conjugate fiber, at a bath ratio of 1: The color yield value (K / S value) according to the CIE 1976 standard can be 14 or more when staining at normal pressure for 40 minutes.

According to an embodiment of the present invention, the polyester-based component may include at least one selected from the group consisting of polyethylene terephthalate, polypropylene terephthalate, polybutylene terephthalate, and polybutylene adipate terephthalate.

The present invention also provides an interior yarn comprising the thermoadhesive composite fiber according to the present invention.

According to an embodiment of the present invention, the interior yarn may be applied to any one of a vehicle seat, a bed sheet, a blind, a curtain, and an interior article.

The polyester composition for thermoadhesive fibers according to the present invention is flexible in adhering, can exhibit soft touch, and has low density, so that a thermoadhesive conjugate fiber having excellent color yield in dyeing under low temperature and low pressure conditions can be realized . The thermosetting conjugate fiber according to the present invention can be widely used for interior sheets, bedclothes, blinds, curtains, interior goods, and the like for interior yarns.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a cross-sectional schematic diagram of a thermally adhesive composite fiber according to an embodiment of the present invention; FIG.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings, which will be readily apparent to those skilled in the art to which the present invention pertains. The present invention may be embodied in many different forms and is not limited to the embodiments described herein.

The polyester composition for thermoadhesive fibers of the present invention will be described.

The polyester composition for thermoadhesive fibers of the present invention comprises an esterified compound in which an acid component containing terephthalic acid and a diol component containing ethylene glycol and 2-methyl-1,3-propanediol are reacted with a polyalkylene glycol And a polycondensated copolyester.

The esterified compound can exhibit thermal adhesion properties even at a low temperature due to the 2-methyl-1,3-propanediol contained in the diol component, and the esterified compound having low temperature thermal adhesion property and the By polycondensation of a poly-alkylene glycol having a chain-like structure, the copolyester of the present invention has excellent adhesion strength at the time of bonding, soft touch and softness, excellent radiation workability, and excellent durability even in a low temperature and low pressure environment .

The acidic component may further include isophthalic acid in an amount of 1 to 15 mol% of the acidic component, thereby lowering the glass transition temperature of the copolyester and improving adhesion strength and soft feel have.

When the isophthalic acid is contained in an amount of less than 1 mol% of the acid component, the effect of decreasing the glass transition temperature of the copolyester, improving the adhesive strength upon bonding and improving the soft touch may not be exhibited. In addition, when the isophthalic acid is contained in an amount exceeding 15 mol% of the acid component, not only the soft touch is reduced but also many side reactants of the cyclic compound are formed by the use of isophthalic acid, .

The 2-methyl-1,3-propanediol contained in the diol component may be contained in the diol component in an amount of 25 to 40 mol%, more preferably 29 to 40 mol%.

When the 2-methyl-1,3-propanediol is contained in an amount of less than 25 mol% of the diol component, the copolyester may have a high bonding temperature, which may be difficult to use for thermally adhesive fibers, It may be difficult to achieve the object of the present invention such that the melting point increases with increasing crystallinity of the copolyester.

When the 2-methyl-1,3-propanediol is contained in an amount of 29 to 40 mol% of the diol component, even when 2-methyl-1,3-propanediol is used alone as the diol component, A melting point lowering effect can be exhibited, and when it is used in combination with isophthalic acid and polyethylene glycol, the melting point can be more effectively lowered and an excellent adhesive strength can be exhibited.

When the diol component contains diethylene glycol other than the naturally occurring amount, the glass transition temperature is rapidly lowered, resulting in deterioration of heat resistance, deterioration of storage stability and stability over time, lowering the melt viscosity of spinning, There is a problem that radioactivity may be remarkably lowered.

In the polyester composition for heat-bondable fibers according to an embodiment of the present invention, the diol component does not substantially contain diethylene glycol, so that the fibers are refracted during the spinning process, the cross-section uniformity is lowered, , And the problem of a sudden decrease in heat resistance (glass transition temperature) can be prevented or minimized.

However, the diethylene glycol can occur naturally in the esterification reaction.

The acid component and the diol component may be polymerized to form an esterified compound at a molar ratio of 1: 1 to 1: 2. If the molar ratio is less than 1: 1, the acidity during polymerization may be excessively high, If the molar ratio exceeds 1: 2, the degree of polymerization may not be increased.

The polymerization of the acid component and the diol component may be carried out under the conditions used in the esterification polymerization reaction commonly used in the art, for example, at 200 to 260 ° C for 150 to 240 minutes at a rate of 40 to 80 rpm But it is not limited thereto.

Next, the copolyesters of the present invention can be prepared by polycondensation of the esterified compounds with polyalkylene glycols.

The polyalkylene glycol may preferably be polyethylene glycol.

More preferably, the polyethylene glycol may have a weight average molecular weight of 400 to 12000, and when the weight average molecular weight of the polyethylene glycol is less than 400, it is difficult to exhibit the desired soft touch and migration effect, The polymerization reactivity is lowered and the thermal stability due to the decrease in the heat resistance of the polymerized product may be poor. Most preferably, the polyethylene glycol may have a weight average molecular weight ranging from 400 to 6000, and accordingly, the soft tactile sensation and the mucous appearance can be exerted, and the effect of preventing or minimizing the deterioration of heat resistance can be further improved.

The polyalkylene glycol may be contained in an amount of 1 to 10% by weight based on the weight of the esterified compound. If the polyalkylene glycol is contained in an amount of less than 1% by weight based on the weight of the esterified compound, it is difficult to exhibit the desired soft touch and migration effect, and the copolyester If it is contained in an amount of more than 10% by weight, the polymerization reactivity is lowered, the thermal stability of the resulting polymer is deteriorated due to the decrease in heat resistance, and the spinning workability is lowered. .

More preferably, the polyalkylene glycol may be contained in an amount of 1 to 5% by weight based on the weight of the esterified compound, so that not only the polycondensation reaction can be more stably maintained, but also the copolyester It is possible to secure a more stable level of heat resistance.

As described above, the esterified compound can exhibit thermal bonding properties even at a low temperature due to the 2-methyl-1,3-propanediol contained in the diol component, and the esterified compound having low- , The copolyester of the present invention is excellent in adhesive strength at the time of bonding, soft at the same time with soft touch and excellent in spinning workability, and can be used in a low-temperature and low-pressure environment And the copolyester is obtained by reacting an acid component of terephthalic acid with a diol component comprising 60 to 71 mol% of ethylene glycol and 29 to 40 mol% of 2-methyl-1,3-propanediol in a molar ratio of 1: 1 to 1: 2, and a polyethylene glycol having a weight average molecular weight of 400 to 6000, which is contained in an amount of 1 to 10% by weight based on the weight of the esterified compound If the polycondensation is prepared, the yeomchakseong, the adhesive strength when bonded in a soft feel, a low temperature and a low pressure environment can be more excellent.

Next, the thermosetting conjugate fiber of the present invention will be described.

The thermally adhesive composite fiber 10 of the present invention comprises a core portion 11 containing a polyester component and a sheath portion 12 comprising a polyester composition for a thermally adhesive fiber according to the present invention, (12).

The polyester component contained in the core portion 11 may include at least one selected from the group consisting of polyethylene terephthalate, polypropylene terephthalate, polybutylene terephthalate and polybutylene adipate terephthalate.

The fineness of the conjugate fiber 10 may be preferably from 1 De to 15 De in order to minimize the problem of deterioration in spinning workability. Since the composition of the polyester composition for thermoadhesive fibers is the same as that described above, detailed description thereof will be omitted.

The composite fibers may be produced by a composite spinning method commonly used in the art, for example, a melt spinning method may be used, but the present invention is not limited thereto.

The thermosetting conjugate fiber according to the present invention is a polyester composition for thermoadhesive fiber having excellent adhesion strength at the time of adhesion, soft and soft touch, excellent spinning workability, and excellent durability even in a low temperature and low pressure environment Is contained in the sheath portion, it is possible to have an excellent adhesive strength of not less than 100 N when measuring the adhesive strength based on the KSM ISO 36 method, and 2% by weight of a dye (C.I. Basic Blue 54), the color yield value (K / S value) according to the CIE 1976 standard, when stained at a bath ratio of 1: 50 at 120 DEG C and atmospheric pressure for 40 minutes, can have an excellent dyeability of 14 or more.

Next, an interior yarn including the thermosetting conjugate fiber according to the present invention will be described. Since the interior yarn includes the thermosetting conjugate fiber according to the present invention, it is possible to dye in a low-temperature and low-pressure environment, thereby remarkably reducing the cost of the dyeing process and securing excellent durability of the interior product by having excellent adhesive strength The soft touch feeling can be excellent. Accordingly, the interior yarn can be applied to any one of a vehicle seat, a bedding, a blind, a curtain, and an interior article.

(Example 1)

Terephthalic acid (TPA), ethylene glycol (EG) and 2-methyl-1,3-propanediol (MPO) were added to the ester reaction tank and reacted at a temperature of 250 ° C by a conventional method to prepare an esterified compound. In the preparation of the esterified compound, the acid component and the diol component were mixed at a molar ratio of 1: 1.5, and the diol component contained 65 mol% of EG and 35 mol% of MPO.

 Polyethylene glycol (weight average molecular weight: 1000) was added in an amount of 2% by weight based on the weight of the produced esterified compound, and then the temperature was elevated to 285 ° C while gradually reducing the pressure to 1.0 Torr or less so that the copolyester ≪ / RTI >

The produced low melting point copolyester was used as a sheath portion, and polyethylene terephthalate was spun at a spinning temperature of 275 DEG C and a spinning speed of 500 mpm using a sheath / core barrel so as to form a core so that the polyester conjugate fiber (fineness: 4de , Length: 51 mm).

(Examples 2 to 14)

Except that at least one of the acid component, the diol component, the content thereof, the polyethylene glycol content and the weight average molecular weight thereof contained in the esterified compound were changed as shown in the following Table 1 Fiber.

(Comparative Examples 1 to 4)

Except that at least one of the acid component, the diol component, the content thereof, the polyethylene glycol content and the weight average molecular weight thereof contained in the esterified compound were changed as shown in the following Table 1 Fiber.

(Experimental Example 1)

The glass transition temperature of the copolyester and the viscosity of the polyester composition prepared in Examples and Comparative Examples were measured and the adhesive strength, color yield, soft touch feeling and radiation workability of the composite fibers prepared in Examples and Comparative Examples were evaluated The results are shown in Table 1 below.

(1) Glass transition temperature measurement

The glass transition temperature (T _g ) of the copolyester prepared in Examples and Comparative Examples was measured using a differential scanning calorimeter (DSC), and the results are shown in Table 1 below. The glass transition temperature was measured at a rate of 20 ° C / min

(2) Viscosity measurement

The copolyester prepared in Examples and Comparative Examples was added to Ortho-Chloro Phenol at a concentration of 0.2 g / 25 ml and then melted at 110 ° C for 30 minutes. The molten solution was incubated at 25 DEG C for 30 minutes and viscosity was measured from an automatic viscometer connected to a CANON viscometer.

(3) Evaluation of adhesive strength

The polyester conjugate fibers prepared in Examples and Comparative Examples were mixed and fused with ordinary polyethylene terephthalate staple fibers using a carding machine and heat-treated at a temperature of 140 ° C with a tenter to obtain a basis weight The adhesive strength was measured by a universal testing machine (UTM) according to the KS M ISO 36 method. The nonwoven fabric was 35 g / m ² , and the width, length, and thickness were 100 mm × 20 mm × 10 mm.

 (4) Evaluation of color yield

The color yield evaluation was performed by dyeing the conjugate fiber for 2 minutes at a temperature of 120 DEG C and a pressure of 40 minutes at a bath ratio of 1:50 for a salt solution containing 2% by weight of a dye (C.I. Basic Blue 54) After measuring the spectral reflectance of the visible fiber (360 to 740 nm, 10 nm interval) of the dyed composite fiber using a colorimetric system of KURABO Co., Ltd. of Japan, the spectral reflectance of the total The K / S value was calculated to evaluate the color yield of the dye.

(5) Soft touch evaluation

The soft touch of the composite fibers was evaluated by sensory test method by a panel composed of 10 peers of the same industry. When the sensory test results showed that more than 8 people were soft, excellent (◎), 6-7 were good, 4 were normal (△), and less than 4 were bad (×).

(6) Evaluation of radiation workability

Radiation workability of composite fibers was evaluated by sensory test method by a panel of 10 peer industry experts based on the degree of threading and uniformity during spinning. When sensory test results showed that more than 8 workers had excellent spinning workability Excellent (◎), 6-7 were good (○), 5 ~ 4 were normal (△), and less than 4 were bad (×).

division Copolyester Poly
s
Terre
Composition Conjugated fiber Esterified compound Polyalkylene
Glycol Tg
(° C) IV
(dl / g) Adhesive strength
(N /
25 mm) color
Yield
(K / S) soft
touch radiation
Workability Acid component Diol component TPA
(mole%) IPA
(mole%) EG
(mole%) MPO
(mole%) DEG
(mole%) PEG
(weight%) weight
Average
Molecular Weight Example 1 100 0 65 35 0 2 200 64 0.640 110 13 △ ○ Example 2 100 0 65 35 0 2 500 64 0.648 117 14 ○ ○ Example 3 100 0 65 35 0 2 1000 63 0.635 132 15 ◎ ◎ Example 4 97 3 65 35 0 2 1000 61 0.648 137 15 ◎ ◎ Example 5 100 0 70 30 0 5 1000 60 0.652 130 18 ◎ ○ Example 6 100 0 70 30 0 9 1000 56 0.651 137 17 ◎ ○ Example 7 100 0 65 35 0 2 5600 61 0.652 146 19 ◎ ◎ Example 8 100 0 65 35 0 2 6600 60 0.651 143 19 ◎ ○ Example 9 100 0 65 35 0 2 11200 58 0.663 140 19 ◎ △ Example 10 100 0 65 35 0 2 13500 51 0.660 Poor polymerization Example 11 100 0 78 22 0 2 1000 70 0.640 89 14 ◎ ◎ Example 12 100 0 73 27 0 2 1000 68 0.648 108 15 ◎ ◎ Example 13 100 0 62 38 0 2 1000 67 0.648 145 17 ◎ ◎ Example 14 100 0 57 43 0 2 1000 66 0.651 128 16 ◎ ○ Comparative Example 1 100 0 50 50 0 2 1000 67 0.628 124 13 ◎ ○ Comparative Example 2 100 0 70 30 0 0 - 73 0.635 92 12 △ ○ Comparative Example 3 100 0 70 30 0 13 1000 46 0.645 Poor radiation Comparative Example 4 97 3 58 35 7 2 1000 57 0.638 145 16 ◎ △

Referring to Table 1, it can be seen that Example 4 containing 3 mol% of IPA in the esterification reaction had better adhesive strength than Example 3 containing no IPA. Further, in the esterification reaction, In Comparative Example 4, it was confirmed that the radiation workability was significantly lowered when the conjugate fiber was spun.

On the other hand, in Comparative Example 2 which does not contain PEG in the polycondensation reaction, it is confirmed that not only the bonding strength and the color yield are remarkably low, but also excellent soft touch feeling can not be realized. On the other hand, Example 6 containing 9 wt% of PEG in the polycondensation reaction shows excellent adhesion strength, color yield, soft touch and radiation workability, whereas Comparative Example 3 containing 13 wt% There was a difficult problem.

Example 2 containing PEG having a weight average molecular weight of 200 in the polycondensation reaction is superior in adhesive strength and color yield and excellent in soft touch feeling than Example 1 having a weight average molecular weight of 500. On the other hand, Example 10 containing PEG having a weight average molecular weight of 13500 had difficulty in polymerization itself, and Example 9 containing PEG having a weight average molecular weight of 11200 had remarkable adhesive strength, color yield and soft touch Excellent, but radiation workability was moderate. On the other hand, Example 8 containing PEG having a weight average molecular weight of 6600 showed not only excellent adhesion strength, color yield and soft touch but also excellent spinning workability.

Further, Example 11 containing 22 mol% of MPO in the esterification reaction was excellent in color yield, soft touch and radiation workability, but had a problem that the adhesive strength was relatively low. On the other hand, it can be confirmed that the adhesive strength of Example 12 containing 27% by mole of MPO was significantly increased as compared with Example 11. Further, it was confirmed that the adhesive strength of Example 13 containing 38 mol% of MPO was significantly higher than that of Example 14 containing 43 mol% of MPO, and the color yield and spinning workability were also superior.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

10: Composite fiber
11: core part
12: Sheth Boo

Claims (17)

An acid component comprising terephthalic acid and a diol component comprising ethylene glycol and 2-methyl-l, 3-propanediol in a molar ratio of 1: 1 to 1: 2 and the esterified compound reacted with the esterified compound By weight, based on the total weight of the composition, of polyethylene glycol containing from 1 to 10% by weight,
The polyethylene glycol has a weight average molecular weight of 400 to 12,000,
Wherein the 2-methyl-1,3-propanediol is contained in an amount of 29 to 40 mol% of the diol component.
The method according to claim 1,
Wherein the diol component does not contain diethylene glycol.
delete delete delete The method according to claim 1,
Wherein the polyethylene glycol has a weight average molecular weight of 400 to 6000.
delete delete delete The method according to claim 1,
Wherein the acid component further comprises isophthalic acid in an amount of 1 to 15 mol% of the acid component.
The method according to claim 1,
Wherein the copolyester comprises an acid component of terephthalic acid, a diol component comprising 60 to 71 mol% of ethylene glycol and 29 to 40 mol% of 2-methyl-1,3-propanediol in a molar ratio of 1: 1 to 1: 2 And a polyethylene glycol having a weight average molecular weight of 400 to 6000, which is contained in an amount of 1 to 10% by weight, based on the weight of the esterified compound, and the esterified compound.
A core portion comprising a polyester-based component; And
A sheath portion including the polyester composition for a thermally adhesive fiber according to Claim 1 surrounding the core portion;
And the thermosetting conjugated fiber.
13. The method of claim 12,
The composite fibers were fused and improved with a polyethylene terephthalate staple fiber in a weight ratio of 1: 1, and then heat treated at 140 ° C to obtain a test piece having a width of 100 mm, a length of 20 mm, and a thickness of 10 mm. 36. A thermo-adhesive composite fiber having an adhesive strength of at least 100 N measured by a universal testing machine (UTM).
13. The method of claim 12,
The composite fibers were dyed at a bath ratio of 1:50 at 120 DEG C and atmospheric pressure for 40 minutes against a dye solution containing 2 wt% of dyes (C.I. Basic Blue 54) based on the weight of the composite fibers, and CIE 1976 (K / S value) of 14 or more.
13. The method of claim 12,
Wherein the polyester-based component comprises at least one selected from the group consisting of polyethylene terephthalate, polypropylene terephthalate, polybutylene terephthalate and polybutylene adipate terephthalate.
An interior yarn comprising the thermoadhesive conjugate fiber according to claim 12.
17. The method of claim 16,
The interior yarn is applied to any one selected from the group consisting of a vehicle seat, a bedclothes, a blind, a curtain, and an interior.

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