JP7081965B2 - Fabric - Google Patents

Description

The present invention relates to a polyester multifilament and a woven fabric capable of obtaining a woven fabric having an excellent texture with a squeaky feeling.

Woven and knitted fabrics made from raw silk have long been used habitually for their high-quality luster, soft swelling, moderate elasticity, excellent texture such as creaking, and comfortable wearing. However, silk products are expensive, and there are many problems such as handling such as washing.

On the other hand, in the field of synthetic fibers as well, efforts have been made to obtain fibers for woven and knitted fabrics that exhibit a high squeaky feeling of raw silk yarn. For example, Patent Document 1 proposes to add a more natural mottled feeling by forming a similar irregular cross-section yarn into a thick and thin structure. Further, Patent Document 2 also proposes a multi-leaf cross-section mixed fiber yarn having a groove in the leaf portion.

If grooves are formed on the fiber surface as in these proposals, the squeakability is certainly improved, but all of them are composite fibers, and the entire periphery of the difficult-to-elute component polymer in the core is surrounded by the easy-eluting polymer. Since the easily-eluting polymer is eluted to improve the ximi property, the manufacturing cost is high, and a large amount of the easily-eluting polymer is discharged in the manufacturing process, so that the manufacturing method has a high environmental load.

JP-A-59-192709 Japanese Unexamined Patent Publication No. 9-228173

The present invention has been made in view of the above background, and an object of the present invention is to provide a polyester multifilament and a fabric capable of obtaining a fabric having a texture excellent in a squeaky feeling.

As a result of diligent studies to achieve the above problems, the present inventors have obtained a polyester multifilament in which the cross-sectional shape of the single fiber is a trilobal cross section and micropores are formed on the fiber surface of the single fiber. It has been found that when the fabric is constructed, it exhibits an extremely excellent texture with a squeaky feeling, and further diligent studies have led to the completion of the present invention.

Thus, according to the present invention, " a fabric made of polyester multifilament.
In the polyester multifilament, the cross-sectional shape of the single fiber is a trilobal cross section, and micropores are formed on the fiber surface of the single fiber, and the micropores formed on the fiber surface of the single fiber. The average length in the minor axis direction is in the range of 0.1 to 1.0 μm, the average length in the major axis direction is in the range of 0.5 to 5.0 μm, and the number of micropores is 10 μm in the fiber axial direction. 5 or more per, the single fiber fineness is in the range of 0.5 to 5.0 dtex, the number of filaments is 12 or more, and the number of filaments is 12 or more.
A woven fabric having a cover factor of CF1200 to 3000 and a basis weight of 100 to 190 g / m ² . Is provided.
At that time, in the polyester multifilament, it is preferable that the variation CV% of the area of the triangle connecting each apex in the trilobal cross section by a straight line is within the range of 5 to 15%.

According to the present invention, a polyester multifilament and a woven fabric that can obtain a woven fabric having an excellent texture with a squeaky feeling can be obtained.

In the polyester multifilament of the present invention, a schematic view of a single fiber cross section is shown, and a triangle ABC in which each apex in the trilobal cross section is connected by a straight line is shown. It is a drawing substitute photograph (2500 times) of the single fiber surface of the polyester multifilament obtained in Example 1. FIG. It is a figure which shows typically the micropores formed in the fiber surface in the polyester multifilament of Example 1. FIG.

The present invention is a polyester multifilament, and the cross-sectional shape of the single fiber is a trilobal cross section, and micropores are formed on the fiber surface of the single fiber.

At that time, the average length of the micropores formed on the fiber surface of the single fiber in the minor axis direction is 0.1 to 1.0 μm, and the average length in the major axis direction is 0.5 to 5. Within the range of 0 μm, the surface of the fiber is lowered in refractive index and the mirror reflection of the incident light is suppressed, so that the fiber after dyeing enables a deep hue and excellent luster, and also gives a feeling of squeaky feeling of the fabric. Can express excellent texture. The number of micropores is preferably 5 or more per 10 μm in length in the fiber axis direction.

Further, when the variation CV% of the area of the triangle connecting each apex in the trefoil cross section is within the range of 5 to 15%, a natural luster is obtained while controlling the non-uniformity in each filament. In addition, it is preferable because the variation in the area can express the excellent texture of the fabric when it is woven and knitted. If the variation CV% is less than 5% or more than 15%, there is a possibility that a natural feeling may be lost due to a glossy feeling and a squeaky feeling in a woven or knitted fabric, and an excellent texture cannot be expressed.

In the polyester multifilament of the present invention, the single fiber fineness is preferably in the range of 0.5 to 5.0 dtex in order to obtain an excellent squeaky feeling. Further, in order to obtain an excellent squeaky feeling, the number of filaments is preferably 12 or more (more preferably 12 to 90).

Further, as the type of polyester, polyethylene terephthalate or polytrimethylene terephthalate is preferable.

Hereinafter, the manufacturing method will be described by taking as an example the case where the polyester multifilament is a polyethylene terephthalate fiber.

First, in polyethylene terephthalate, the main repeating unit is ethylene terephthalate, terephthalic acid is the main acid component, and ethylene glycol is the main glycol component.

Such polyethylene terephthalate may have a small amount (usually 30 mol% or less) of a copolymerization component, if necessary.

Examples of the bifunctional carboxylic acid other than the terephthalic acid used include isophthalic acid, naphthalindicarboxylic acid, diphenyldicarboxylic acid, diphenoxyetanedicarboxylic acid, β-hydroxyethoxybenzoic acid, and P-oxybenzoic acid, 5. -Aromatic, aliphatic and alicyclic bifunctional carboxylic acids such as sodium sulfoisophthalic acid, adipic acid, sebacic acid and 1,4-cyclohexanedicarboxylic acid can be mentioned. Examples of the diol compound other than the glycol include aliphatic, alicyclic, aromatic diol compounds such as cyclohexane-1,4-dimethanol, neopentyl glycol, bisphenol A and bisphenol S, and polyoxyalkylene glycol. Can be given.

The polyethylene terephthalate may be synthesized by any method. For example, terephthalic acid and ethylene glycol are directly esterified, terephthalate lower alkyl ester such as dimethyl terephthalate is subjected to an ester exchange reaction with ethylene glycol, or terephthalic acid is reacted with ethylene oxide. The first-stage reaction to produce a glycol ester of terephthalic acid and / or a low polymer thereof, and the second-stage reaction in which the reaction product of the first stage is heated under reduced pressure and subjected to a polycondensation reaction until a desired degree of polymerization is achieved. Manufactured by reaction.

Further, various stabilizers, ultraviolet absorbers, thickening branching agents, matting agents, colorants, various other improving agents and the like may be blended in polyethylene terephthalate, if necessary.

It is important that the polyethylene terephthalate contains the metal-containing phosphorus compound (a) and the alkaline earth metal compound (b) represented by the following general formulas.

式中、Ｒ１およびＲ２は一価の有機基である。この一価の有機基は具体的にはアルキル基、アリール基、アラルキル基または［（ＣＨ_２）ｌＯｋ］Ｒ３（ただし、Ｒ３は水素原子、アルキル基、アリール基またはアラルキル基、ｌは２以上の整数、ｋは１以上の整数）等が好ましく、Ｒ１とＲ２とは同一でも異なっていてもよい。Ｍはアルカリ金属またはアルカリ土類金属であり、Ｌｉ、Ｎａ、Ｋ、Ｍｇ、Ｃａ、Ｓｒ、Ｂａが好ましく、特にＣａ、Ｓｒ、Ｂａが好ましい。ｍはＭがアルカリ金属のとき１であり、Ｍがアルカリ土類金属のとき１／２である。

In the formula, R1 and R2 are monovalent organic groups. The monovalent organic group is specifically an alkyl group, an aryl group, an aralkyl group or [(CH ₂ ) lOK] R3 (where R3 is a hydrogen atom, an alkyl group, an aryl group or an aralkyl group, and l is 2 or more. An integer, k is an integer of 1 or more) and the like are preferable, and R1 and R2 may be the same or different. M is an alkali metal or an alkaline earth metal, and Li, Na, K, Mg, Ca, Sr, and Ba are preferable, and Ca, Sr, and Ba are particularly preferable. m is 1 when M is an alkali metal and 1/2 when M is an alkaline earth metal.

If a phosphorus compound in which R1 and / or R2 is replaced with a metal (particularly an alkali metal or an alkaline earth metal) is used instead of the metal-containing phosphorus compound (a), the fine pores generated in the obtained polyester fiber are large. As a result, the desired squeaky feeling cannot be obtained, and the fibril resistance is also inferior.

In order to produce the metal-containing phosphorus compound (a), it is easy to heat-react the corresponding positive phosphate ester (mono, di or bird) with a predetermined amount of the corresponding metal compound in the presence of a solvent. can get. At this time, it is most preferable to use glycol used as a raw material for polyethylene terephthalate as the solvent.

The alkaline earth metal compound (b) used in combination with the metal-containing phosphorus compound (a) is not particularly limited as long as it reacts with the metal-containing phosphorus compound (a) to form an insoluble salt in polyethylene terephthalate. Not of alkaline earth metal acetates, oxalates, benzoates, phthalates, organic carboxylates such as stearate, borates, sulfates, silicates, carbonates, bicarbonates. Examples thereof include inorganic acid salts, halides such as chlorides, chelate compounds such as ethylenediamine tetraacetic acid complex salts, hydroxides, oxides, alcoholates such as methylate, ethylate and glycolate, and phenolates. In particular, organic carboxylates, halides, chelate compounds, and alcoholates that are soluble in ethylene glycol are preferable, and organic carboxylates are particularly preferable. The above alkaline earth metal compound (b) may be used alone or in combination of two or more.

When the metal-containing phosphorus compound (a) and the alkaline earth metal compound (b) are added, the amount of the metal-containing phosphorus compound (a) used and the metal-containing phosphorus are used in order to give a squeaky feeling to the obtained polyethylene terephthalate fiber. It is preferable to specify the ratio of the amount of the alkaline earth metal (b) used to the amount of the compound (a) used. That is, if the amount of the metal-containing phosphorus compound (a) added is too small, the color depth becomes insufficient, and as the amount is increased, the color depth increases, but if it is too large, the color depth is no longer significantly improved. On the contrary, the abrasion resistance durability is deteriorated, it becomes difficult to obtain a polyester having a sufficient degree of polymerization and a softening point, and there is a possibility that a trouble that yarn breakage occurs frequently at the time of spinning may occur. Therefore, the amount of the metal-containing phosphorus compound (a) added is preferably in the range of 0.5 to 3 mol%, and more preferably in the range of 0.6 to 2 mol% with respect to the acid component constituting the polyethylene talephthalate. .. Further, if the amount of the alkaline earth metal compound (b) added is less than 0.5 times the molar amount of the amount of the metal-containing phosphorus compound (a) added, the deep color property of the obtained polyester fiber becomes insufficient. In addition, the polycondensation rate may decrease, making it difficult to obtain a polyester having a high degree of polymerization, and the softening point of the produced polyester may be significantly reduced. On the contrary, if the alkaline earth metal compound (b) in an amount exceeding 1.2 times by mole with respect to the metal-containing phosphorus compound (a) is added, coarse particles may be generated. Therefore, the amount of the alkaline earth metal compound added to the metal-containing phosphorus compound is preferably in the range of 0.5 to 1.2 times mol, and more preferably in the range of 0.5 to 1.0 times mol.

It is preferable that the metal-containing phosphorus compound (a) and the alkaline earth metal compound (b) are added to the polyethylene terephthalate reaction system without reacting in advance. By doing so, insoluble particles can be produced in polyethylene terephthalate in a uniform ultrafine particle state. If the metal-containing phosphorus compound (a) and the alkaline earth metal compound (b) were previously reacted externally to form insoluble fine particles and then added to the polyethylene terephthalate reaction system, the dispersibility of the insoluble particles in polyethylene terephthalate was obtained. However, the effect of improving the color depth of the obtained polyethylene terephthalate fiber may not be recognized because the coarse agglomerated particles are contained.

The addition of the metal-containing phosphorus compound (a) and the alkaline earth metal compound (b) can be carried out in any order at any stage until the synthesis of polyethylene terephthalate is completed. However, if only the metal-containing phosphorus compound (a) is added at a stage where the reaction of the first stage has not been completed, the completion of the reaction of the first stage may be hindered, and the alkaline earth metal compound (b). ) Is added before the end of the first stage reaction, and when this reaction is an esterification reaction, coarse particles are generated during this reaction, and when this reaction is a transesterification reaction, the reaction proceeds abnormally quickly. Since it may cause a bumping phenomenon, in this case, it is preferably about 20% by weight or less. It is preferable that at least 80% by weight of the alkaline earth metal compound (b) and the total amount of the metal-containing phosphorus compound (a) are added after the stage where the reaction of the first stage of the synthesis of polyethylene terephthalate is substantially completed. .. Further, when the metal-containing phosphorus compound (a) and the alkaline earth metal compound (b) are added at a stage where the reaction of the second stage proceeds too much, the particles tend to be aggregated and coarsened. It is preferable that the ultimate viscosity of the reaction mixture in the second stage reaction is before reaching 0.3.

The above-mentioned metal-containing phosphorus compound (a) and alkaline earth metal compound (b) may be added at one time, divided into two or more times, or continuously.

In addition, any catalyst can be used for the first-stage reaction, but some of the alkaline earth metal compounds (b) have the catalytic ability for the first-stage reaction, particularly the ester exchange reaction. When such a compound is used, it is not necessary to use a separate catalyst, and this alkaline earth metal compound can be added before or during the reaction in the first stage and can also be used as a catalyst. Since it may cause a bumping phenomenon as described above, it is preferable that the amount used is less than 20% by weight of the total amount of the alkaline earth metal compound to be added.

As described above, the metal-containing phosphorus compound (a) and the alkaline earth metal compound (b) are added to the polyethylene terephthalate reaction system without prior reaction, and then the synthesis of polyethylene terephthalate is completed. It is possible to obtain polyethylene terephthalate which has a high degree of polymerization, a high softening point, a good passability in a thread-making process, and can give a fiber having an excellent squeaky feeling.

In addition, various additives such as matting agents such as titanium dioxide, heat stabilizers, defoaming agents, color stabilizers, flame retardants, antioxidants, ultraviolet absorbers, infrared absorbers, etc. are included in the polymer. Includes additives such as fluorescent whitening agents, plasticizers, impact resistant additives, or reinforcing agents such as montmorillonite, bentonite, hectrite, plate iron oxide, plate calcium carbonate, plate boehmite, or carbon nanotubes. Needless to say, it may be.

Next, a spinneret having a trilobal cross section is used to spin and stretch the fabric by a conventional method, and if necessary, the fabric is made into a fabric. Is formed. At that time, the alkali weight loss rate is preferably in the range of 5 to 40% (more preferably 10 to 30%) with respect to the weight of the polyethylene terephthalate fiber. If the alkali weight loss rate is less than 5%, fine pores may not be sufficiently formed on the fiber surface of the polyethylene terephthalate fiber.

In the polyester multifilament thus obtained, the intrinsic viscosity [η] F of the fiber is an important factor affecting the strength elongation property, toughness, and tear resistance of the polyester multifilament, and the range thereof. Is preferably 0.60 or more and 0.80 or less, and more preferably 0.60 or more and 0.70 or less. If this [η] F is less than 0.60, the tear resistance of the fabric may be insufficient. On the other hand, when [η] F exceeds 0.80, the silk-reeling property may be significantly deteriorated, and the process passability may be significantly deteriorated due to fluff and thread breakage.

Next, the cloth of the present invention is a cloth made by using the polyester multifilament. It is preferable that the polyester multifilament is contained in an amount of 40% by weight or more based on the weight of the fabric.

In such a cloth, the structure of the woven or knitted fabric is not limited and may be knitted or woven by a usual method. For example, as the weaving structure, a three-pronged structure such as plain weave, velvet weave, satin weave, a changing structure, a changing structure such as a changing diagonal weave, and a single double structure such as a vertical double weave and a horizontal double weave. An example is velvet. Further, as the knitted fabric, a half structure, a half base structure, a satin structure and the like using two or three reeds are preferably exemplified.

In particular, when the fabric is a woven fabric, it is preferable that the cover factor CF of the woven fabric is in the range of 1200 to 3000 because an excellent squeaky feeling can be obtained.

However, the cover factor CF is defined by the following formula.
CF = (DWp / 1.1) ^1/2 x MWp + (DWf / 1.1) ^1/2 x MWf
However, DWp is the total warp fineness (dtex), MWp is the warp weft density (book / 2.54 cm), DWf is the total weft fineness (dtex), and MWf is the weft weft density (book / 2.54 cm).

Next, when the fabric is dyed, excellent deep color property is obtained due to the fine pores formed on the fiber surface of the polyethylene terephthalate fiber, and there is no difference in dyeing and dyeing.

The fabric of the present invention is subjected to various processes such as embossing, coloring print, water repellent treatment, ultraviolet shielding agent, antibacterial agent, deodorant, insect repellent, phosphorescent agent, retroreflecting agent, negative ion generator and the like. May be additionally applied.

Since the polyester multifilament described above is contained in the fabric thus obtained, the feeling of squeaking is excellent.

Here, the basis weight of the fabric is preferably 200 g / m ² or less (more preferably 100 to 190 g / m ² ).

The fabric is suitably used as clothing such as women's black formal clothing, party dresses, men's suits, slacks, and sports clothing.

Next, the present invention will be described in detail with reference to examples, but the present invention is not limited thereto. In addition, each physical property in an Example was measured by the following method.
(1) Intrinsic Viscosity The resin or fiber was dissolved in a mixed solvent of phenol and ortodichlorobenzene (volume ratio 6: 4), and measured at 35 ° C. using an Ostwald viscometer.
(2) Fine pores on the fiber surface A side photograph was taken with a scanning electron microscope from a direction perpendicular to the fiber axis at a magnification of 3500 times, and on the fiber surface excluding the length of 10% from both ends of the fiber width in the side photograph. At any 20 locations, the length in the minor axis direction is 0.1 to 1 μm, which exists at 80% of the fiber width excluding the above 10% length in the direction perpendicular to the fiber axis, in the major axis direction. The number of micropores having a length of 0.5 to 10 μm was counted and converted per 10 μm in length, and the average value at these 20 locations was taken as the number of micropores.
(3) Texture of the fabric Gloss and squeaky feeling The obtained fabric was evaluated by 10 panelists consisting of weaving, knitting, and dyeing engineers on a 10-point scale, and the total score was evaluated.
80 points or more: 〇50-79 points: △
49 points or less: ×
29 points or less: XX
(4) Metsuke The basis weight (g / m ² ) was measured by JIS L-1096 (8.3).

[Practical example 1]
In the esterification reaction tank, 86 parts of terephthalic acid and 40 parts of ethylene glycol were subjected to an esterification reaction according to a conventional method to obtain an oligomer. 86 parts of terephthalic acid and 40 parts of ethylene glycol were continuously supplied to this oligomer over 65 minutes, and an esterification reaction was carried out at 245 ° C. Then, 20 minutes after adding 0.045 part of antimony trioxide, an oligomer having an equimolar amount equal to that of the oligomer produced from the additionally supplied terephthalic acid and ethylene glycol was sent to the polycondensation reaction tank. Immediately after the completion of the liquid feeding, 0.5 mol% of calcium acetate was added to the polycondensation reaction tank with respect to the acid component in the polymer. After a further 5 minutes, 0.6 mol% of phenylphosphonic acid was added to the polycondensation reaction tank with respect to the acid component in the polymer. After that, the temperature was raised to 290 ° C., a polycondensation reaction was carried out under a high vacuum of 0.03 kPa or less to obtain a polyester chip having an intrinsic viscosity of 0.65 dL / g, and then this chip was dried at 140 ° C. for 6 hours. did.

The tip is melted with a molten extruder, the polymer is extruded from the spout discharge hole at a spinning temperature of 290 ° C, passed through a cooling delay zone having an atmospheric temperature of 200 to 250 ° C, and then cooled and solidified and oiled at 1000 m / m /. min. The undrawn yarn was taken up at the above speed, and the obtained undrawn multifilament was drawn 3.8 times, and heat-treated and entangled to obtain a polyester multifilament.

Then, the polyester multifilament was used to prepare a woven fabric having the following structure.
Structure: Plain weave warp / weft density: 170 / 25.4 mm / 140 / 25.4 mm
Fabric basis weight: 70 g / m ²
The obtained woven fabric raw machine was subjected to a scouring, a preset, 10% alkali weight reduction treatment, and a dyeing step by a conventional method, and then heat-treated under predetermined conditions.

[Examples 2 to 4]
It was carried out in the same manner as in Example 1 except that it was carried out as described in Table 1.

[Comparative Examples 1 to 3]
It was carried out in the same manner as in Example 1 except that it was carried out as described in Table 2.

According to the present invention, a polyester multifilament and a woven fabric capable of obtaining a woven fabric having an excellent texture with a squeaky feeling are provided, and the industrial value thereof is extremely large.

A: Long-axis direction of micropores formed on the fiber surface B: Short-axis direction of micropores formed on the fiber surface C: Fiber cross section

Claims (2)

A woven fabric made of polyester multifilament.
In the polyester multifilament, the cross-sectional shape of the single fiber is a trilobal cross section, and micropores are formed on the fiber surface of the single fiber, and the micropores formed on the fiber surface of the single fiber. The average length in the minor axis direction is in the range of 0.1 to 1.0 μm, the average length in the major axis direction is in the range of 0.5 to 5.0 μm, and the number of micropores is 10 μm in the fiber axial direction. 5 or more per, the single fiber fineness is in the range of 0.5 to 5.0 dtex, the number of filaments is 12 or more, and the number of filaments is 12 or more.
A woven fabric having a cover factor of CF1200 to 3000 and a basis weight of 100 to 190 g / m ² . The fabric according to claim 1, wherein in the polyester multifilament, the variation CV% of the area of the triangle connecting each apex in the trilobal cross section by a straight line is in the range of 5 to 15%.

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