KR20140131968A - Polyamide fiber and method for producing same - Google Patents

Polyamide fiber and method for producing same Download PDF

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KR20140131968A
KR20140131968A KR1020147026183A KR20147026183A KR20140131968A KR 20140131968 A KR20140131968 A KR 20140131968A KR 1020147026183 A KR1020147026183 A KR 1020147026183A KR 20147026183 A KR20147026183 A KR 20147026183A KR 20140131968 A KR20140131968 A KR 20140131968A
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polyamide
yarn
package
fibers
winding
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KR1020147026183A
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KR101918049B1 (en
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켄타로 타카기
켄지 이토
타케오 야마모토
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도레이 카부시키가이샤
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides

Abstract

The present invention relates to a polyamide fiber having a specific structure and having a strength of not less than 3.5 cN / dtex and an elongation of 70 to 150%, wherein the polyamide fiber is produced by discharging molten polyamide from a spinneret, The yarn is cooled and solidified by the cooling wind, the yarn for tanning is attached to the yarn, the yarn is taken thereafter, and the yarn is again wound up. And the following conditions (a) and (b) are satisfied.
(a) The distance from the outlet of the detention to the attachment of the emulsion for smoking is 500 to 1,500 mm
(b) the draw speed is not less than 3300 m / min and not more than 4300 m / min, and the take-up speed is 0.8 to 1.2 times
The present invention provides a polyamide fiber which has a high degree of denseness and which is capable of real processing rich in variation, and a method for producing the polyamide fiber excellent in productivity.

Description

FIELD OF THE INVENTION [0001] The present invention relates to a polyamide fiber,

TECHNICAL FIELD The present invention relates to a high-purity polyamide fiber excellent in workability and a method for producing the same.

Polyamide fibers typified by polyamide 6 fibers and polyamide 66 fibers, and polyester fibers typified by polyethylene terephthalate fibers and polybutylene terephthalate fibers are excellent in mechanical properties and dimensional stability. Therefore, these fibers are widely used not only for medical applications but also for interior, interior materials for automobiles, and industrial materials.

The polyester fiber is produced by high-speed production, so that the fiber structure (in particular, the orientation and crystallization of the molecular chains) can be controlled and the product can be wound with good productivity. There is an elongation as one of the characteristics that characterize the fiber structure. By varying the elongation, various yarns are obtained from the fibers. For example, a false twist yarn giving a winding property and a stretch false yarn having a thick portion and a thin portion expressing neck joints. There are also fusion welders. In addition, there is a compound singer who made the characteristic of the texture by having the difference of the thread length of these fibers by combining the high - Among such polyester fibers, there are processing yarns rich in variations to give added value, and polyester fibers are widely used.

On the other hand, polyamide fibers have the following problems even if it is attempted to control the fiber structure by a manufacturing process such as polyester fiber. There is a case where the fibers are swollen at the time of the take-up winding due to the progress of the orientation crystallization due to the humidity of the environment, and as a result, the yarn in the take-up package is shifted and the yarn ruptures. Therefore, the stretchability of the polyamide fibers that can be stably wound is limited. As a result, there is a limitation in obtaining fibers for yarn processing for imparting added value, and polyamide yarns have been lacking in variety until now.

For this reason, there has been a demand for a high-definition polyamide fiber which imparts winding properties during stable dressing in order to obtain polyamide processed yarn rich in variation.

Various proposals have been made so far to improve the elongation of polyamide fibers. For example, there has been proposed a highly-oriented polyamide fiber containing a specified amount of polyamide 610 and / or polyamide 612 having a specific range of relative viscosity to polyamide 6 (see Patent Document 1).

Further, high-molecular-weight polymeric fibers in which polyesters such as polyethylene terephthalate and polylactic acid are dispersed in polyamide 6 have been proposed (see Patent Document 2).

It has also been proposed that a polyamide having a glass transition point of 40 占 폚 or higher is wound up at a low speed and is not stretched or stretched to 2.5 times or less to obtain a high-tint polyamide (see Patent Document 3).

Japanese Patent Application Laid-Open No. 2002-339164 Japanese Patent Application Laid-Open No. 2005-206961 Japanese Patent Application Laid-Open No. 2004-27456

In the method described in Patent Document 1, since orientation crystallization is suppressed, high-purity polyamide fiber can be obtained, but the durability as a final product is poor, which is not suitable for medical use. In the method described in Patent Document 2, high crystallinity polyamide fibers can be obtained because orientation crystallization is suppressed. However, in the case of using this fiber as a final product, peeling of the interface between the phase of the polyamide and the phase of the polyester occurs, and the problem of deterioration of the abrasion resistance has been a problem. Also, in the method described in Patent Document 3, it is possible only in two steps of spinning and stretching, and the productivity is very poor, which is not suitable for industrialization. In addition, since this fiber has an elongation of more than 220%, it becomes a very unstable crystal structure, so that it has a problem that the dimension changes with time.

It is an object of the present invention to provide a polyamide fiber and a production method thereof excellent in productivity by obtaining a processed yarn having a high degree of shininess and rich in variations by the present invention.

In order to solve the problems, the present invention has the following configuration.

(1) Polyamide fibers having a strength of 3.5 cN / dtex or more and an elongation of 70 to 150%, which are polyamides which are polymers of the structural formula A shown below or polyamides which are polymers of the structural formula B;

Figure pct00001

In the structural formula A, l is 9 to 12,

In formula (B), (m + n) / 2 is 6-12.

(2) The polyamide fiber according to (1), wherein the polyamide is a polymer of the structural formula (B).

(3) The polyamide fiber according to (1), wherein the polyamide is a polymer of the structural formula A.

(4) A cheese-shaped package comprising any one of the above-mentioned polyamide fibers, and having a deburring ratio expressed by the following formula (I) of 10% or less.

B (%) = {(WB-WS) / WS} x 100 (I)

(B: Bulling ratio, WB: Maximum width of package (mm), WS: Width of starting winding of package (mm)).

(5) A method in which a molten polyamide is discharged from a spinneret to form a yarn, the yarn is cooled and solidified by a cooling wind, the spinning oil is adhered to the yarn, and the yarn is wound thereon and the yarn is wound Wherein the polyamide fiber is produced by a method comprising the following steps (a) and (b).

(a) The distance from the outlet of the detention to the attachment of the emulsion for smoking is 500 to 1,500 mm

(b) the draw speed is not less than 3300 m / min and not more than 4300 m / min, and the take-up speed is 0.8 to 1.2 times

(6) A composite processed yarn comprising the polyamide fibers described in any one of the above and fibers having an elongation of less than 70%.

(7) A fabric for putting the polyamide fiber according to any one of the above.

(Effects of the Invention)

According to the present invention, it is possible to provide a polyamide fiber which can be wound with excellent productivity, has a high degree of shininess, can be subjected to real processing with abundant variety, and a production method thereof.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a cross-sectional view of two types of polyamide fibers of the present invention. Fig.
2 is a conceptual view showing an example of a process for producing a synthetic fiber according to the present invention.
3 is a cross-sectional view of the cheese-shaped package of the present invention according to the present invention.
4 is a schematic view showing a manufacturing process of a composite working yarn of an embodiment of the present invention.

Hereinafter, the polyamide fibers of the present invention will be described in more detail.

As the polymer used for the polyamide fiber of the present invention, a so-called hydrocarbon group is a polymer of the structural formula A or the polymer of the structural formula B, which is connected to the main chain through an amide bond.

Figure pct00002

The polymer of the structural formula A is mainly a polymer composed of units represented by the structural formula A and the polymer of the structural formula B is a polyamide which is a polymer mainly composed of units represented by the structural formula B. [ In Structural Formula A, l is 9-12. That is, it means that [CH 2 ] / [NHCO] in the structural formula A, that is, the number of methylene groups per one amide group is 9 to 12. Examples of structural formula A include polyamide 11 (the number of methylene groups per amide group is 10) and polyamide 12 (the number of methylene groups per amide group is 11). Here, the polymer may be a copolymer of different types of structural units included in the category of structural formula A.

In formula B, (m + n) / 2 is 6-12. Means that the number of methylene groups per amide group in the structural formula B is 6 to 12. Examples of the structural formula B include polyamide 410 (the number of methylene groups per amide group 6), polyamide 510 (the number of methylene groups per one amide group is 6.5), polyamide 610 (the number of methylene groups per amide group is 7) 612 (the number of methylene groups per amide group is 8). Or may be a copolymer of heterologous structures included in the category of the structural formula B.

When the number of methylene groups per one amide group is in the range of the present invention, there is a tendency that the polyamide having the structural formula A and the polyamide having the structural formula B have the following characteristics.

If the number of methylene groups per one amide is less than a specific amount, amide bonds in the polymer are increased and the moisture absorption rate is increased. Until the polyamide fiber is wound up, the spinning oil or moisture in the air is absorbed to a large extent, and as a result, the yarn is swollen by moisture and thus the stable spinning is difficult. When the number of methylene groups per one amide exceeds a specific amount, the melting point of the polymer is lowered. Further, the amide bond in the polyamide is reduced. Polyamide fibers are characterized by hygroscopicity and dyeability of fibers, but the expected hygroscopicity is difficult to obtain, and dyeing becomes difficult, narrowing the range of application to medical applications. Further, the intermolecular hydrogen bonds due to the amide bonds are reduced, and the strength of the fibers tends to be lowered.

Of these two types of polyamides, polyamides substantially consisting of the structural formula B are preferable, and (m + n) / 2 is more preferably 6 to 7 in view of heat resistance and dyeability. Examples of such polyamides include polyamide 410, polyamide 510, and polyamide 610.

The polyamide, which is a polymer of the structural formula A, can be prepared from an aminocarboxylic acid or cyclic amide as a raw material. The polyamide of formula B can be prepared from dicarboxylic acid and diamine as raw materials. Hereinafter, these raw materials are collectively referred to as monomers. As the monomer, a petroleum-derived monomer, a biomass-derived monomer, a mixture of a petroleum-derived monomer and a biomass-derived monomer is not limited. However, in recent years, it has been desired to include a biomass-derived monomer as a raw material in view of the attention of environment-adaptable polymers. It is more preferable that at least 50 mass% of the monomers constituting the polyamide are monomers obtained by using biomass from the viewpoint of excellent environmental adaptability. The monomer unit derived from this biomass is preferably 75% by mass or more, and more preferably 100% by mass.

Examples of such monomers include sebacic acid derived from biomass. This can be manufactured from castor oil. There is also pentane diamine derived from biomass. This can be produced by fermenting glucose.

The polyamide of the present invention may be copolymerized with other components within a range that does not impair the effect of the present invention. That is, as the high molecular weight substance substantially constituted by the polymer consisting of the units represented by the structural formula A and the structural formula B, a component which generates a unit other than the unit represented by the structural formula A and the structural formula B may be copolymerized in the range of not lowering the effect of the present invention can do. For example, a small amount of a caproamide unit or a hexamethylene adipamide unit can be copolymerized with the polyamide. Such a case may also be considered as being within the scope of the polymer of the present invention since the effect of the present invention is achieved. In the polyamide of the present invention, the units represented by the structural formula A or the units represented by the structural formula B preferably contain 90 mol% or more of the total amide units, respectively. As the copolymerization component, copolymerizable components which generate units other than the unit represented by the structural formula A include aminocarboxylic acids, lactams, amines (diamines, monoamines, etc.), aliphatic monocarboxylic acids , An aliphatic dicarboxylic acid, an aromatic dicarboxylic acid, and the like. Examples of the copolymerizable component that generates a unit other than the unit represented by the structural formula B include an aminocarboxylic acid and a lactam, and diamines and dicarboxylic acids that generate units other than the units represented by the structural formula B, and the like.

The viscosity of the polyamide of the present invention is preferably a polymer having a relative viscosity of 98% sulfuric acid at 25 DEG C of 2.0 to 3.0. When the relative viscosity of 98% sulfuric acid is small, the molecular weight of the polyamide becomes low, and it becomes difficult to obtain sufficient strength when the fiber is made into a fiber. However, if the relative viscosity is too large, the extrusion pressure of the molten polymer during spinning becomes high. In addition, the extrusion pressure rise during spinning is significantly delayed, and the jaws must be quickly replaced.

The polyamide fiber of the present invention may further contain various inorganic additives and organic additives such as a polish eliminator, a flame retardant, an antioxidant, an ultraviolet absorber, an infrared absorber, a nucleating agent, a fluorescent whitening agent, an antistatic agent, Antimicrobial agents (silver zeolite, zinc oxide, etc.), and the like. If the above-mentioned additives can be copolymerized with polyamide, they may be copolymerized. The sum of the contents of these additives is preferably in the range of 0.001 to 10 mass% with respect to the polyamide.

In addition, the cross-sectional shape of the short fibers of the polyamide fiber of the present invention may show not only a round cross section, but also a variety of different cross-sectional shapes such as flat, Y, T, hollow, cross-sectional shapes shown in Fig. The shape of the fibers may be multifilament or monofilament.

The polyamide fiber of the present invention has an elongation of 70 to 150%. When the elongation is low, the processable conditions for processing the obtained polyamide fibers become narrow, and it becomes difficult to obtain added value for the obtained fibers. For example, in the case of a false-twist yarn obtained by performing a twist process after stretching to make a thick portion and a thin portion, narrowing of the range of stretching conditions makes it difficult to sufficiently obtain a difference in the fineness of the thick portion and the thin portion. As a result, it is difficult to express the expected neck coordination when fabric or knitted fabric is used. Further, in the case of a composite processed yarn obtained by interlacing a part of the low yarn yarn, it is difficult to sufficiently obtain the yarn length difference, and it becomes difficult to express a feeling of satisfaction that can be satisfied when the knitted fabric is used. In addition, when the fibers are excessively elongated, the non-soft portions are increased in the structure of the fibers, and water tends to crystallize when water is introduced into a large amount of non-soft portions. As a result, the fiber length is increased during winding, and the yarn is stretched in the package, so that the yarn in the winding package is displaced and ruptured, so that it becomes difficult to wind it stably. In addition, fibers with too large elongation tend to have a large number of non-fibers in the fiber structure. When the wastes are wound up, water enters the nondominant part which is present in large quantity, and it becomes easy to crystallize. When the fibers are stretched after being stretched, the yarn layer in the wound package is displaced and ruptured, which makes it difficult to stably wind the fibers. Also, the washing fastness in the final product using fibers with too large elongation is reduced. As a result of considering these problems, the optimum elongation is 70 to 150%. And more preferably 80 to 150%.

The strength of the polyamide fiber of the present invention is preferably 3.5 cN / dtex or more. By increasing the strength, an effect can be obtained on the quality of the final product and the sacrifice. In the case of a small size, not only the high-order permeability at the time of actual processing, weaving and unfolding deteriorates but also durability in the final product is hardly obtained. The more preferable strength is 4.0 cN / dtex or more.

The total fineness of the polyamide fibers of the present invention can be appropriately set according to the use, but is preferably 10 to 230 dtex, and more preferably 10 to 200 dtex. The monofilament fineness can be appropriately set according to the application, but is preferably 0.5 to 10 dtex, more preferably 0.5 to 5 dtex in view of flexibility when processed into a fabric.

The polyamide fibers of the present invention are produced by general melt spinning as a basic spinning method, and the production process thereof is not particularly limited as long as the polyamide fibers of the present invention can be obtained. However, it can be produced by the following production method.

The molten polyamide is discharged from the spinneret to form a yarn, the yarn is cooled and solidified by the cooling wind, the spinning oil is adhered to the yarn, the yarn is then drawn, and the yarn is wound again.

This method will be described in detail with reference to Fig. 2 is a conceptual diagram showing an example of a process for producing a fiber according to the present invention.

The molten polyamide is metered with the gear pump 1, extruded, discharged from the spinneret 2, and polyamide is treated as a fibrous yarn. The cooling air is sprayed by the cooling device 3 such as a chimney to cool the yarn to a temperature near room temperature to solidify the yarn of the polyamide. The lure is fed to the lubrication device (4) and is concentrated. Then, the yarn is entangled with the interlocking nozzle device 5 and is carried by the first felt rollers 6, passed through the second felt rollers 7, and then wound up by the winding device 8.

In the method for producing a polyamide fiber of the present invention, the distance from the outlet of the nipping to the attachment of the repellent agent is preferably 500 mm or more and 1500 mm or less. Preferably 500 mm or more and 1200 mm or less, further preferably 500 mm or more and 1000 mm or less. If this distance is short, the emulsion is adhered before the completion of draft stretching, and there is a possibility that the strength of the resulting fiber may be lowered. If the distance is large, shrinkage due to excessive drafting during winding occurs, winding tends to occur during winding, and the yarn drum is not pulled out, so that stable production tends to be difficult.

The polyamide used in the polyamide fibers of the present invention has a lower absorption rate than the general absorption rate of polyamide 6 of 1.8% in view of the ratio of the number of amide groups to the number of methylene groups. In general polyamide 6, the glass transition temperature is lower than the room temperature due to moisture absorption before lubrication by the oil supply device 4, and the polymer chain can freely move, so that the tension increase is small even if the yarn runs in the air. However, the polyamide yarns of the present invention have a lower glass transition temperature lower than that of the polyamide 6, and the glass transition point is usually 25 ° C or higher at room temperature. Above the glass transition temperature, the polymer chain in the fiber can not move and the tensile force generated by the yarn traveling in the air is great. Therefore, even if the distance from the spinneret 2 to the oil refueling device 4 to which the repellent agent is attached is the same, the yarn tension of the polyamide fiber of the present invention becomes larger. As a result, as the tensile force is increased, the stretching of the accompanying air stream applied to the first felt rollers 6 is increased, so that shrinkage occurs after being wound on the drum, which tends to result in difficulty in stable production due to the occurrence of winding knot. Therefore, by shortening the distance from the spinneret 2 to the lubricant supply device 4 for adhering the tanning agent, and increasing the tensile force applied to the yarn at a temperature above the glass transition temperature, the polyamide fiber of the present invention is obtained . Since the polyamide 610 of the present invention, for example, polyamide 610 has a higher Young's modulus than polyamide 6, the tension of yarn tends to be increased until it is discharged from the spinneret 2 and attached to the emulsion . As described above, since the stretching applied up to the first felt rollers 6 is a factor, the polyamide fibers are also obtained from the spinneret 2 to the lubricant feeding device 4 It is preferable to shorten the distance between the two.

For this reason, the distance from the spinneret to the attachment of the emulsion for outlet use is preferably not less than 500 mm and not more than 1,200 mm, and more preferably not less than 500 mm and not more than 1,000 mm.

It is preferable that the radial emulsion imparted by the oil feed device 4 is a water based emulsion. When the functional emulsion is added, the temperature of the glass transition point of the polyamide is lowered by the moisture contained in the emulsion at the stage during the sacrifice, and the decrease of the yarn tension between the oil feed device 4 and the entangled nozzle device 5 So that the stretching between the lubricant feeding device 4 and the interlocking nozzle device 5 is suppressed and the winding knot is reduced.

In the production process of the polyamide fiber of the present invention, it is preferable that the take-in speed is in the range of 3300 m / min to 4300 m / min. The winding speed is preferably 0.8 to 1.2 times the drawing speed. In the case of the manufacturing method shown in FIG. 2, the take-off speed means the peripheral speed of the first felt rollers 6. Further, the winding speed is the peripheral speed of the winding device 8.

The value obtained by dividing the take-up speed and the take-up speed by the take-up speed indicates the total amount of turn, which is an index of the orientation of the polymer. When the total stretching amount is too small, that is, when the pulling speed is small, and when the numerical value obtained by dividing the pulling speed and the winding speed is larger than 1.2 times, the degree of orientation of the fibers is low and the fiber spinning agent or moisture in the air is excessively absorbed , And as a result, the yarn is swollen and can not be stabilized. In addition, when the total elongation amount is too large, that is, when the drawing speed (the peripheral speed of the first felt roller 6) exceeds 4300 m / min or the numerical value obtained by dividing the drawing speed and the winding speed is less than 0.8 times, So that a rewinding knot occurs and stable production can not be performed. Preferably, the pulling speed is in the range of 3300 m / min to 4000 m / min, and the winding speed is in the range of 0.8 to 1.2 times the pulling speed. More preferably not less than 3300 m / min and not more than 3800 m / min, and the winding speed is 1.0 to 1.2 times the pulling speed.

By setting the lubricating position, the take-up speed and the winding speed in this range, stable production can be achieved without swelling in the spinning and winding-up knot, and a satisfactory cheese-shaped package can be obtained.

The cheese-shaped package made of the polyamide fiber of the present invention preferably has a deburring ratio of 10% or less. (WB-WS) / (WB-WS) / (WB-WS) / (WB-WS) WS} × 100. Fig. 3 is a side sectional view schematically showing the cheese-shaped package of the present invention according to the present invention, showing a state in which a yarn B is wound around a paper tube A. Fig.

When the packing ratio exceeds 10%, there arises a problem that it becomes difficult to fix the packing at a predetermined place due to the expansion of the end face of the package when wrapped in a carton case or a pallet. In addition, even if the package can be packed, there arises a problem that the package end face and the wrapping material of the wrapping material due to the friction between the package end face and the package are damaged during the transportation (disconnection of the single yarn and separation of the single yarn). More preferably, it is 8% or less.

The cheese-shaped package made of the polyamide fiber of the present invention is particularly effective when the amount of fibers is 3 kg or more, particularly when the package is wound up, particularly when the package is 4.5 kg or more. The upper limit is not limited, but usually 7.5 kg or less is used.

The polyamide fibers of the present invention can be used singly as fabric bags, but they are more preferably used as fabric bags through a processing chamber. Examples of the working room include a false twisted yarn for imparting a winding property and a stretchable false twist yarn having a thick portion and a thin portion for expressing a neck air tightness and a fusing false twist yarn. In addition, a composite yarn such as a composite yarn which is characterized by having a feeling by providing a yarn length difference by mixing the polyamide fiber yarn of the present invention and the low yarn filament yarn may be mentioned. In the composite yarn, the elongation of the low elongation yarn is preferably less than 70%, more preferably 30 to 50%. Further, in the case of the composite working such as the polyamide fiber yarn of the present invention and the composite yarn or composite false yarn in which one or more other yarns are combined, they may be combined with the same material or may be combined with other materials. The manufacturing method may be performed simultaneously or separately.

Examples of the fiber structure (usually cloth) using the processed yarns from the polyamide polyamide fibers and polyamide fibers of the present invention include sports casual wear such as shirts and jackets, pants, coats, innerwear of gentleman / wife medical care, camisole, And can be used for medical applications such as legs, knitwear, stockings, socks and the like. It can also be used for medical materials such as cups and pads in underwear. It can also be used for interior applications such as curtains, carpets, mats, furniture, and other industrial materials.

Example

The present invention will be described in detail in the following examples. The following methods were used for the measurement method in the examples.

[How to measure]

A. Relative Viscosity of Sulfuric Acid

0.25 g of the sample was dissolved in an amount of 1 g based on 100 ml of sulfuric acid at a concentration of 98% by mass, and the dropping time (T1) at 25 캜 was measured using an Oswald-type viscometer. Subsequently, the dropping time (T2) of sulfuric acid only at a concentration of 98% by mass was measured. The ratio of T1 to T2, that is, T1 / T2, was defined as the relative relative viscosity of sulfuric acid.

B. Intrinsic Viscosity [IV]

(IV) obtained by dissolving 0.8 g of the sample polymer in 10 ml of orthochlorophenol (hereinafter abbreviated as OCP) and calculating the relative viscosity [? R] using an Ostwald viscometer at 25 占 폚 according to the following equation.

The relative viscosity [ηr] = η / η 0 = (t × q) / (t 0 × q 0)

Intrinsic viscosity [IV] = 0.0242? R + 0.2634

However, η: viscosity of the polymer solution, η 0: Viscosity of OCP, t: falling time in seconds of the solution, q: Density (g / ㎤), t 0 of the solution: fall time (sec), q 0 of OCP : Density of OCP (g / cm3).

C. Melting point (Tm)

Using a differential scanning calorimeter DSC-7 manufactured by Perkin-Elmer, 20 mg of a sample polymer is sampled. The temperature of the first scan is raised from 20 DEG C to 270 DEG C at a temperature raising rate of 20 DEG C / minute and held at a temperature of 270 DEG C for 5 minutes. Thereafter, the temperature is lowered from 270 DEG C to 20 DEG C at a cooling rate of 20 DEG C / min. After being maintained at a temperature of 20 DEG C for 1 minute, the temperature is raised from 20 DEG C to 270 DEG C at a temperature raising rate of 20 DEG C / minute as a second scanning. The temperature of the endothermic peak observed at that time was defined as the melting point.

D. Fineness

The sample was wound around the frame at a height of 1.125 m and wound up 200 times. The sample was dried with a hot-air drier (105 ± 2 ° C. × 60 minutes), and the mass of the tuft was weighed with a balance Calculated the fineness. The process water content was 4.5% for polyamide 6, 2.5% for polyamide 610, 3.0% for polyamide 510 and 1.2% for polyamide 12. The measurement was carried out four times, and the average value was determined as the fineness. The value obtained by dividing the obtained fineness by the number of filaments was taken as a single fiber fineness.

E. Strength and elongation

The samples were measured under the constant-rate extensional conditions indicated in JIS L1013 (Test method for chemical fiber filament yarn, 2010) by "TENSILON" (registered trademark), UCT-100 manufactured by Orientech. The elongation was obtained from the elongation at the point showing the maximum strength in the tensile strength-elongation curve. Also, the strength was determined by dividing the maximum strength by the fineness. The measurement was carried out ten times, and the average value was determined as the strength and elongation.

F. Boiling water shrinkage

The obtained polyamide fibers were wound twenty times with a tread coiler having a circumferential length of 1.125 m to form a skein, and the length L 0 was obtained under a load of 0.09 cN / dtex. Then, it is treated for 30 minutes in a no-load and low-humidity water and then air-dried. Subsequently, the length LB after the treatment is obtained under a load of 0.09 cN / dtex, and is calculated by the following equation.

Boiling water shrinkage percentage (%) = [(L 0 -L 1 ) / L 0 ] × 100

G. Cassette letters

Five subjects were compared and evaluated according to the following criteria. The sample of Comparative Example 8 was used as a comparison target.

Excellent: There is a lot of feeling.

Sheep: There is a feeling of drowsiness.

Normal: No background feeling (equivalent to Comparative Example 8)

Poor: There is no sense of roughness (Thinner than Comparative Example 8)

H. only package rate

The package rate obtained when one ton was radiated was calculated as follows.

Package rate (%) = [D 1 / D 0 ] × 100

D 0 : The maximum number of theoretical packages

D 1: 1 ton of the actual number of packages obtained when the emission

(Example 1)

Polyamide 610 (relative sulfuric acid viscosity of 2.67, melting point: 225 占 폚) was used and melt spinning was continuously carried out by the spinning device shown in Fig. 2 to obtain polyamide fibers. The process is as follows. First, the polyamide 610 was charged into a radiator and melted at a spinning temperature of 270 DEG C, the polymer was weighed (35.7 g / min) by the gear pump 1, discharged, And discharged from the surface of the spinneret 2 having a hole with a discharge hole diameter of 0.20 mm and a hole hole length of 0.5 mm with 68 holes to obtain a yarn. The yarn tank was cooled with air by the uniflored cooling device 3 to solidify it, and was refueled by the oil supply device 4. Further, the oil supply device was installed at a position 800 mm from the side of the spinneret. The peripheral speed of the first felt roller 6 is taken to 4094 m / min, the peripheral speed of the second felt roller 7 is set to 4094 m / min, did. The draw ratio is 1.0. Then, a winding speed of 4000 m / min was wound up to obtain a 6 kg cheese-shaped package made of nylon 610 fibers of 96 decitex and 68 filaments. Swelling in the winding drum and winding-up knot do not occur during spinning, so that the yarn can be produced stably. In addition, a plurality of cheese-shaped packages were produced, and as a result, the package ratio was 100%. The evaluation results of the obtained fibers are shown in Table 1.

(Example 2)

A cheese-shaped package of 6 kg of multifilament was obtained under the same conditions as in Example 1, except that the position of the oil supply device was set at a position of 1200 mm from the face of the spinneret. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was 95%. The evaluation results of the obtained fibers are shown in Table 1.

(Example 3)

A 6 kg cheese-shaped package of multifilament was obtained under the same conditions as in Example 1 except that the position of the oil supply device was set at a position of 1500 mm from the spinneret surface. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was only 90%. The evaluation results of the obtained fibers are shown in Table 1.

(Example 4)

The same as in Example 1 except that the peripheral speed of the first felt rollers 6 was 4264 m / min, the peripheral speed of the second felt rollers 7 was 4264 m / min, the drawing magnification was 1.0 and the winding speed was 4200 m / A 6 kg cheese-shaped package of multifilament was obtained. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was 100%. The evaluation results of the obtained fibers are shown in Table 1.

(Example 5)

The same conditions as in Example 1 were used except that the peripheral speed of the first felt rollers 6 was 3839 m / min, the peripheral speed of the second felt rollers 7 was 3839 m / min, the draw ratio was 1.0 and the take-up speed was 3800 m / To obtain a 6 kg cheese-shaped package of multifilament. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was 100%. The evaluation results of the obtained fibers are shown in Table 1.

(Example 6)

The same as in Example 1 except that the peripheral speed of the first felt rollers 6 was 3722 m / min, the peripheral speed of the second felt rollers 7 was 4094 m / min, the drawing magnification was 1.1 and the winding speed was 4000 m / min As a result, a multifilament and a 6 kg cheese-shaped package were obtained. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was 95%. The evaluation results of the obtained fibers are shown in Table 1.

(Example 7)

The same conditions as in Example 1 were used except that the peripheral speed of the first felt rollers 6 was 3321 m / min, the peripheral speed of the second felt rollers 7 was 3819 m / min, the draw ratio was 1.15, To obtain a 6 kg cheese-shaped package of multifilament. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was 95%. The evaluation results of the obtained fibers are shown in Table 2.

(Example 8)

The same conditions as in Example 1 were used except that the peripheral speed of the first felt rollers 6 was 3327 m / min, the peripheral speed of the second felt rollers 7 was 3660 m / min, the drawing magnification was 1.05 and the winding speed was 3600 m / To obtain a 6 kg cheese-shaped package of multifilament. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was 95%. The evaluation results of the obtained fibers are shown in Table 2.

(Example 9)

The polymer was weighed (23.6 g / min) with the gear pump 1 and discharged under the same conditions as in Example 1 except that 24 holes of holes having a discharge hole diameter of 0.30 mm and a hole length of 0.75 mm were discharged from the spinneret Two package packages of 6 kg of multifilament with a total fineness of 64 decitex and 24 filaments were obtained. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was 100%. The evaluation results of the obtained fibers are shown in Table 2.

(Example 10)

A total fineness of 96 decitex was obtained under the same conditions as in Example 1, except that the discharge hole was discharged from the spinneret 2 having 20 holes having a hole diameter of 0.20 mm and a hole length of 0.50 mm, A 6 kg cheese-shaped package of 20 filaments of multifilament was obtained. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was only 90%. The evaluation results of the obtained fibers are shown in Table 1.

(Example 11)

A polymer was weighed (16.2 g / min) with the gear pump 1 and discharged under the same conditions as in Example 1 except that the spinning nozzle 2 having 68 holes of a discharge hole diameter of 0.20 mm and a hole length of 0.50 mm was discharged A total package size of 44 decitex, 34 filament multifilament, 6kg cheese-shaped package was obtained in two packages. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was 100%. The evaluation results of the obtained fibers are shown in Table 2.

(Example 12)

Except that polyamide 12 (sulfuric acid relative viscosity of 2.20, melting point: 180 占 폚) was melted at a spinning temperature of 250 占 폚 and was guided to a spinneret 2 heated to 250 占 폚. 6 kg of the cheese-shaped package. It was possible to produce it very stably without causing swelling and winding knot in spinning. The package rate was 100%. The evaluation results of the obtained fibers are shown in Table 2.

(Example 13)

The same procedure as in Example 1 was repeated except that polyamide 510 (melting point: 216 占 폚) having a sulfuric acid relative viscosity of 2.62 was used and melted at 250 占 폚 and guided to a spinneret 2 heated to 250 占 폚. Shaped cheese package. It was possible to produce it very stably without occurrence of winding knot during spinning. The package rate was 100%. The evaluation results of the obtained fibers are shown in Table 2.

Figure pct00003

Figure pct00004

(Comparative Example 1)

As a result of winding in the same manner as in Example 1 except that the position of the oil supply device was set at a position of 1800 mm from the spinneret surface, a winding knot occurred and the package could not be taken out of the winding device. As a result, a multifilament cheese-shaped package could not be obtained and stable production could not be achieved.

(Comparative Example 2)

As a result of attempting coiling under the same conditions as in Example 1 except that the position of the oil supply device was set at 300 mm from the spinning nozzle surface, the yarn tension from the attachment of the oil agent to the interlocking nozzle device 5 was lowered, (6). As a result, a cheese-shaped package of a multifilament could not be obtained and stable production could not be achieved.

(Comparative Example 3)

The same conditions as in Example 1 were used except that the peripheral speed of the first felt rollers 6 was 4592 m / min, the peripheral speed of the second felt rollers 7 was 4592 m / min, the draw ratio 1.0, To obtain a multifilament cheese-shaped package. A winding knot frequently occurred during spinning. It was possible to remove the package from the winding device and obtained a multi-filament, 6 kg cheese-shaped package. The package rate was 40%, and stable production was not possible. Further, the obtained multifilament had an elongation of 63% and a strength of 4.9 cN / dtex, and high degree of elongation was not exhibited. The resulting cheese-shaped package had a deburring rate of 12.0%, and could not be packed in a predetermined position of the carton case or the pallet.

(Comparative Example 4)

The same conditions as in Example 1 were used except that the peripheral speed of the first felt rollers 6 was 3108 m / min, the peripheral speed of the second felt rollers 7 was 4040 m / min, the draw ratio 1.3, To obtain a multifilament. A winding knot frequently occurred during spinning. It was possible to remove the package from the winding device and obtained a 6 kg cheese-shaped package of multifilament. The package rate was only 50%, and stable production was not possible. Further, the elongation of the obtained fiber was 60% and the strength was 5.2 cN / dtex, and high degree of elongation was not exhibited. Further, the resulting cheese-shaped package had a deburring ratio of 12.5%, and could not be packed in a predetermined place of the carton case or the pallet.

(Comparative Example 5)

As a result of attempting coiling under the same conditions as in Example 1 except that polyamide 6 (sulfuric acid relative viscosity of 2.62, melting point: 220 占 폚, methylene group number of 1: 5) was used, swelling of the fiber due to moisture absorption occurred, A deviation of the yarn layer occurred, and a multifilament and a cheese-shaped package could not be obtained, and stable production could not be performed.

From the results of Examples 1 to 13 and Comparative Examples 1 to 5 shown in Tables 1 and 2, it can be understood from the results of the inventions of the production method of polyamide fibers that a very stable production is possible without swelling and winding- .

(Examples 14 to 16)

Polytrimethylene terephthalate having an intrinsic viscosity [IV] of 1.40 and polyethylene terephthalate having an intrinsic viscosity [IV] of 0.51 were melted at a weight ratio of 50:50 and a spinning temperature of 275 ° C, and the mixture was melt-extruded . After cooling the discharge yarn, the yarn was cooled by a drawing roller heated at 55O < 0 > C at 1200 m / min and wound on a stretching roller heated at 4200 m / min to 155 DEG C to perform stretching and heat treatment. . Thereafter, it was pulled by a third roller of unheated heat at a stretch rate of -4.5% (speed: 4011 m / min), wound by a fourth roller of 4011 m / min in an unheated state and wound by a winder to obtain a polyester of 33 decitex 12 filaments Shaped composite multi-filament.

Polyamide 610 multifilaments of 96 dtex 68 filaments obtained in Examples 1, 5 and 9 were respectively prepared as nodules. A polyester composite multifilament (33 dtex, 34% elongation, 3.7 cN / dtex) of 33 decitex 12 filaments attached to the cheese-shaped package shown above was prepared for examination. A composite processed yarn of 129 dtex 88 filaments was obtained using the composite yarn processing machine (THK, Aikisai Sakusho Co., Ltd.) shown in Fig.

This specific method will be described in Fig. First, superfine yarn was fed from the superabsorbent package 10 through the superfine feed roller 11. This yarn was introduced into the combustible heater 13 while being twisted by the twister 12 in the downward direction and was set in a heat setting manner and the superfluous yarn was picked up by the super use pick up roller 15 and supplied to the nozzle 16 again. On the other hand, the polyamide fibers were taken from the examination package 9 to the examination drawing roller 14 and fed to the nozzle 16. The sucking and examination yarns fed to the nozzle 16 were entangled with the nozzles 16. The entangled yarn becomes a processed yarn, which is wound on the winding device 18 via the take-up roller 17. Then, a composite processed yarn 19 was obtained.

For the specific machining conditions, the machining speed was 250 m / min, the burn-in magnification was 1.22 times, the heater temperature was 190 占 폚, the D / Y ratio was 1.6 times, and the twister was a three-axis type.

Polyester composite multifilaments forming the deep portion are located at the center of the composite processed yarn, while the polyamide 610 multifilament forming the superficial portion has a difference in thread length from the polyester composite multifilament I have. The composite processed yarn was placed in a planar state in a free state, and a difference in the length of the yarn was observed. Compared to the yarns of Examples 7, 5 and 1, the yarn of the yarn of the Example 7 has the highest yarn length difference and the yarn of the Example 1 has the lowest yarn length. By making the letter of the obtained composite processed yarn and evaluating the feeling of touch, the yarn length difference was increased and the feeling was increased. The evaluation results are shown in Table 3.

(Examples 17 to 18)

A polyamide 12 multi-filament of 96 decitex-68 filaments obtained in Example 12 and a polyamide 510 multifilament of 96 decitex-68 filaments obtained in Example 13 were used in the same manner as in Example 14 except that the polyamide- And a composite processed yarn of 129 dtex 88 filaments was obtained. As a result, a composite letter was prepared in the same manner as in Example 14. The evaluation results are shown in Table 3.

(Comparative Example 7)

The polyamide 610 multifilament of 96 dtex 68 filament obtained in Comparative Example 4 was subjected to composite processing in the same manner as in Example 14 to obtain a composite processed yarn of 129 dtex 88 filaments. As a result, a composite letter was prepared in the same manner as in Example 14. The evaluation results are shown in Table 3.

(Comparative Example 8)

The circumferential speed of the first felt rollers 6 was pulled at 4545 m / min, and the temperature of the second felt rollers 7 was set to 60 m / min. A peripheral speed of 4545 m / min, a draw ratio of 1.0, and a take-up speed of 4500 m / min to obtain a polyamide 6 multifilament of 96 dtex 68 filaments. Further, the fineness was 96.0 dtex, elongation was 60%, and the strength was 4.5 cN / dtex.

Polyamide 6 multifilaments of 96 dtex 68 filaments obtained were subjected to composite processing in the same manner as in Example 14 to obtain a composite processed yarn of 129 dtex 88 filaments. As a result, a composite letter was prepared in the same manner as in Example 14. The evaluation results are shown in Table 3.

Figure pct00005

From the results shown in Table 3, it can be seen that a letter having a good background feeling can be obtained by using the polyamide fiber of the present invention.

1: Gear pump
2: spinning detention
3: Cooling unit
4: Lubrication device
5: interlocking nozzle device
6: first goather roller
7: second goather roller
8: Winding device
A: Paper tube
B:
9: Screening Package
10: Supercharged package
11: Feed rollers for second use
12: Flammable heater
13: Twister
14: Feed roller for examination
15: Draw rollers for seconds
16: Nozzle
17:
18: retractor
19: Composite Processor

Claims (7)

A strength of 3.5 cN / dtex or more, and an elongation of 70 to 150%, the polyamide being a polymer of the structural formula A or the polyamide being a polymer of the structural formula B shown below.
Figure pct00006

[In formula A, l is 9 to 12,
(M + n) / 2 in the structural formula B is 6 to 12] The method according to claim 1,
Wherein the polyamide is a polymer of the formula B. The method according to claim 1,
Characterized in that the polyamide is a polymer of the structural formula A. A cheese-shaped package comprising the polyamide fiber according to any one of claims 1 to 3 and having a deburring ratio expressed by the following formula (I) of 10% or less.
B (%) = {(WB-WS) / WS} x 100 (I)
(B: Bulge ratio, WB: Maximum width of package (mm), WS: Width of starting winding of package (mm)). A method for producing a polyester resin composition, comprising the steps of discharging a molten polyamide from a spinneret to form a yarn, cooling and solidifying the yarn by cooling air, adhering the spinning oil to the yarn, winding the yarn thereafter, A method for producing a polyamide fiber according to any one of claims 1 to 3, wherein the following conditions (a) and (b) are satisfied.
(a) The distance from the outlet of the detention to the attachment of the emulsion for smoking is 500 to 1,500 mm
(b) the draw speed is not less than 3300 m / min and not more than 4300 m / min, and the take-up speed is 0.8 to 1.2 times A composite fabric comprising a polyamide fiber according to any one of claims 1 to 3 and a fiber having an elongation of less than 70%. A fabric according to any one of claims 1 to 3, which comprises the polyamide fiber.
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