TWI595127B - Polyamide fiber and method for producing the same - Google Patents

Description

Polyamide fiber and its manufacturing method

The present invention relates to a high elongation polyamide fiber excellent in workability and a method for producing the same.

Polyamide fiber represented by polyamine 6 fiber or polyamide 66 fiber, or polyester fiber represented by polyethylene terephthalate or polybutylene terephthalate, which has mechanical properties or dimensional stability Excellent sex. Therefore, these fibers are used not only for clothing applications, but also for indoor, vehicle interior materials, industrial materials, and the like.

The polyester fiber is produced by using high-speed yarn production, and controls the fiber structure (especially molecular chain alignment and crystallization) to make it productive and coiled. The characteristic elongation is one characteristic of the fiber structure. By varying the elongation, various processed yarns can be obtained from the fibers. For example, it is provided with a crimped false twisted yarn, and further has a stretched false twist yarn which expresses a rough portion and a thin portion of the texture. Also, there is a fusion of false crepe. Further, there is also a composite false twist yarn having a woven fabric structure in which a yarn of high elongation is combined with a yarn of low elongation and has a yarn length difference of the fibers. Among such polyester fibers, polyester fibers are widely used because of the added value and the richly processed yarn.

On the other hand, the polyamide fiber has the following problems even if it is controlled by the same manufacturing process as the polyester fiber. By the progress of the alignment crystallization by the environmental humidity, the fibers are swollen during the winding of the yarn, and as a result, the yarn layer separation and the yarn breakage of the take-up package occur. Therefore, the range of elongation of the polyamide fiber which can be stably taken up is limited. As a result, there is a limitation in obtaining a yarn for imparting additional value to the yarn for processing, and the polyamide processed yarn is in a state of lack of change.

Therefore, in order to obtain a polyamine-processed yarn which is rich in variation, it is desired to impart a high elongation polyamide fiber which is capable of imparting windability at the time of customizing the yarn.

So far, in order to increase the elongation of polyamide fibers, various proposals have been made. For example, a polyamide fiber having a high elongation of polyamine 610 and/or polyamide 612 having a specific viscosity in a specific range of a specific amount of polyamine 6 is disclosed (see Patent Document 1).

Further, a polymer alloy fiber having a high elongation of a polyester represented by polyethylene terephthalate or polylactic acid is dispersed in the polyamide 6 (see Patent Document 2).

Further, it has been disclosed that polyamine which has a glass transition temperature of 40 ° C or higher at a low speed is not stretched, or is stretched by 2.5 times or less, thereby obtaining a polyamide having a high elongation (see Patent Document 3).

Prior technical literature

Patent literature

Patent Document 1 Japanese Patent Laid-Open Publication No. 2002-339164

Patent Document 2 Japanese Patent Laid-Open Publication No. 2005-206961

Patent Document 3 Japanese Patent Laid-Open Publication No. 2004-27456

The method described in Patent Document 1 suppresses the alignment crystallization, and obtains a polyamide having a high elongation, but the durability of the final product is deteriorated, which is disadvantageous for the use of the clothing. According to the method described in Patent Document 2, a polyamide fiber having a high elongation due to inhibition of alignment crystallization can be obtained. However, when the fiber is used as a final product, the interface between the polyamide phase and the polyester phase is peeled off, and the abrasion resistance is deteriorated. Further, the method described in Patent Document 3 is divided into two steps of spinning and stretching, and the productivity is extremely poor, which is not advantageous for industrialization. Further, the fiber has an elongation of 220% or more, and it has a very unstable crystal structure, and there is a problem of dimensional change over time.

The present invention provides a polyamide fiber having a high elongation and thereby obtaining a processed yarn having a rich variation, and a method for producing the same.

In order to solve the problem, the present invention is constituted by the following.

(1) A polyamide fiber which is a polyamine which has a polymer of the structural formula A shown below, or a polyamine of a polymer of the structural formula B, and has a strength of 3.5 cN/dtex or more and elongation. The rate is 70~150%;

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

In the structural formula B, (m+n)/2 is 6 to 12.

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

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

(4) A cheese-shaped package comprising the polyamide fiber of any one of the above, and having a bulge of 10% or less as expressed by the following formula (I) B(%)={(WB-WS)/WS}×100......(I)

(Where B is the expansion ratio, WB is the maximum width of the package (mm), and WS is the width at which the package starts to be rolled up (mm)).

(5) A method for producing a polyamide fiber, which is a method for producing a polyamide fiber according to any one of the above (a) and (b), characterized in that the molten polyamine is discharged from a nozzle And the yarn is formed, the yarn is cooled and solidified by the cooling air, and after the yarn is attached to the spinning oil, the yarn is recovered and the yarn is further wound; (a) from the nozzle outlet to the spinning oil The distance from the agent is 500 mm or more and 1500 mm or less.

(b) The recovery rate is 3300 m/min or more and 4300 m/min or less, and the coiling speed is 0.8 to 1.2 times the recovery speed.

(6) A composite processed yarn comprising the polyamide fiber of any one of the above, and a fiber having an elongation of less than 70%.

(7) A fabric comprising the polyamide fiber of any one of the above.

According to the present invention, it is possible to provide a polyamide fiber which is excellent in productivity and which has a high elongation and a variable yarn processing and a method for producing the same.

1‧‧‧Gear pump

2‧‧‧Spinning nozzle

3‧‧‧Cooling device

4‧‧‧ oil supply unit

5‧‧‧Interlaced nozzle device

6‧‧‧1st godet

7‧‧‧2nd godet

8‧‧‧Winding device

A‧‧‧paper tube

B‧‧‧ yarn

9‧‧‧ core yarn packaging

10‧‧‧sheath packaging

11‧‧‧feeding rolls for sheath yarns

12‧‧‧ crepe machine

13‧‧‧false heater

14‧‧‧Recycling roller for core yarn

15‧‧‧Recycling roller for sheath yarn

16‧‧‧ nozzle

17‧‧‧Recycling roller

18‧‧‧Winding device

19‧‧‧Composite processed yarn

Fig. 1 is a cross-sectional view showing two examples of cross-sectional yarns of different shapes of the polyamide fibers of the present invention.

Fig. 2 is a conceptual diagram showing an example of a manufacturing process of the synthetic fiber of the present invention.

Figure 3 is a cross-sectional view of a flat cylindrical package of the present invention.

Fig. 4 is a schematic view showing a manufacturing procedure of a composite processed yarn according to an embodiment of the present invention.

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

The polymer used as the polyamide fiber of the present invention is a polyamine which is a polymer of the structural formula A or a polymer of the structural formula B in which a hydrocarbon group is a main chain via a guanamine bond.

The polymer of the structural formula A is a polymer mainly composed of a unit represented by the structural formula A, and the polymer of the structural formula B is a polyamine which is a polymer mainly composed of a unit represented by the structural formula B. .

In Structural Formula A, l is 9-12. That is, it means that [CH2]/[NHCO] in the structural formula A, that is, the number of methylene groups per one amine group is from 9 to 12. In the case of the structural formula A, the polyamine 11 (the number of methylene groups per one amine group is 10) or the polyamide 12 (the number of methylene groups per one amine group is 11). Here, the polymer may also be copolymerized with different building blocks comprising the scope of structural formula A.

In the structural formula B, (m+n)/2 is 6 to 12. That is, it means that the number of methylene groups per one of the amine groups in the structural formula B is from 6 to 12. In the case of the structural formula B, there are polyamine 410 (the number of methylene groups per one amine group is 6), and polyamine 510 (the number of methylene groups per one amine group is 6.5), Polyamine 610 (the number of methylene groups per one amide group is 7) and polyamido 612 (the number of methylene groups per one amide group is 8). Copolymerization of different configurations including the scope of Structural Formula B can also be used.

Polyamide having structural formula A and polycondensation having structural formula B When the number of methylene groups per one of the amine groups is outside the range of the present invention, the following characteristics tend to be obtained.

If the number of methylene groups per one indoleamine is less than a specific amount, then the poly The indole bond in the compound becomes more and the moisture absorption rate becomes larger. When the polyamide fiber is wound up, the spinning oil or the moisture in the air is absorbed in a large amount, and as a result, the yarn is swollen by moisture, and it becomes difficult to stabilize the spinning. If the number of methylene groups per one of the guanamine exceeds a certain amount, the melting point of the polymer decreases. also. The indole bond in the polyamine is less. The polyamide fiber is characterized by hygroscopicity or dyeability of fibers. However, since it is difficult to obtain the desired hygroscopicity and dyeing becomes difficult, the application range for the use of the clothing becomes narrow. Further, the guanamines are bonded to each other and the hydrogen bonding between the molecular chains is reduced, and the fiber strength tends to decrease.

Among the above two polyamines, it is preferred to The polyamine which is composed of the above is more preferably (m+n)/2 or 6 to 7 in terms of heat resistance or dyeability. As the soluble polyamine, for example, polyamine 410, polyamine 510, and polyamine 610 can be exemplified.

Polyamide of the polymer of formula A, which can be an aminocarboxylate An acid or a cyclic guanamine is produced as a raw material. The polyamine of the formula B can be produced by using a dicarboxylic acid and a diamine as a raw material. Hereinafter, the raw materials are referred to as monomers. The single system is not limited to a petroleum-derived monomer, a biomass-derived monomer, a mixture of a petroleum-derived monomer and a biomass-derived monomer, and the like. Among them, recently, in view of the fact that the polymer corresponding to the environment is attracting attention, it is preferred to contain a monomer derived from biomass as a raw material. In terms of excellent environmental adaptability, it is better 50% by mass or more of the monomer constituting the polyamine is a monomer obtained by using a raw material. The monomer unit derived from the raw material is preferably 75 mass% or more, more preferably 100 mass%.

As a monomer of this kind, it can be mentioned that it is derived from the raw material. acid. It can be made from castor oil and also has glutaric acid derived from raw biomass. It can be made by fermenting glucose.

The polyamine of the present invention does not degrade the effect of the present invention. Within the range, it can be copolymerized with other ingredients. That is, the polymer composed of the unit represented by Structural Formula A and Structural Formula B substantially constitutes a high molecular polymer, and is formed within the range in which the effect of the present invention is not lowered, and the formation of Structural Formula A and Structural Formula B is shown. The components of the unit other than the unit are copolymerized. For example, the above polyamine is copolymerized with a small amount of a caproamide unit or a hexamethylene adipamide unit or the like. In this case, since the effect of the invention can still be achieved, it can be regarded as the category of the polymer of the present invention. In the polyamine of the present invention, the unit represented by Structural Formula A or the unit represented by Structural Formula B preferably contains 90 mol% or more of the total guanamine unit, respectively. The copolymerization component is a copolymerization component which is a unit other than the unit represented by the structural formula A, and is an aminocarboxylic acid, an intrinsic amine, or an amine which is not a unit of the structural formula A. An amine, a monoamine or the like), an aliphatic monocarboxylic acid, an aliphatic dicarboxylic acid, an aromatic dicarboxylic acid or the like. Examples of the copolymerization component of the unit other than the unit represented by the structural formula B include an aminocarboxylic acid or an indoleamine, and a diamine or a dicarboxylic acid which forms a unit other than the unit represented by the structural formula B.

The viscosity of the polyamine of the present invention is preferably 25 ° C 98% sulfuric acid has a relative viscosity of 2.0 or more and 3.0 or less. If 98% When the relative viscosity of sulfuric acid is small, the molecular weight of polyamine is low, and it is difficult to obtain sufficient strength as a fiber. However, conversely, if the relative viscosity is too large, the molten polymer extrusion pressure at the time of spinning becomes high. In turn, the pressure in the spinning rises too early and is too significant, and the nozzle has to be replaced early.

Moreover, the polyamide fibers of the present invention may contain various inorganic substances. Additives or organic additives, such as: matting agents, flame retardants, antioxidants, UV absorbers, infrared absorbers, crystal nucleating agents, fluorescent whitening agents, antistatic agents, moisture absorbents (polyvinylpyrrolidone, etc.) , antibacterial agents (silver zeolite, zinc oxide, etc.) and the like. If the above additives are copolymerized with polyamine, they may also be copolymerized. The sum of the contents of the additives is preferably in the range of 0.001 to 10% by mass based on the polyamine.

Further, the cross-sectional shape of the single fiber of the polyamide fiber of the present invention The shape is not only a circular cross section, but also a cross-sectional shape of various shapes such as a flat shape, a Y shape, a T shape, a hollow shape, and a profile type as shown in FIG. 1 . Further, the type of the fiber may be a multifilament or a monofilament.

The polyamine fiber of the present invention has an elongation of 70 to 150%. If the elongation is low, the workable conditions at the time of processing the obtained polyamide fiber are narrowed, and it is difficult to obtain added value to the obtained fiber. For example, when false twisting is performed after the thickness is stretched and the false twisted yarn is obtained, the range of the stretchable condition becomes narrow, and it becomes difficult to sufficiently obtain the difference in fineness between the thick portion and the thin portion. As a result, when a woven fabric or a knitted fabric is formed, the desired texture becomes difficult to express. Further, when a composite processed yarn obtained by interlacing a low elongation yarn is used, it is difficult to sufficiently obtain a yarn length difference, and when it is a knitted fabric, it is difficult to express a satisfactory fabric structure. Further, in the fiber-based fiber structure in which the elongation is too large, the amorphous portion is increased, and the yarn is taken up. At the time, the amorphous portion which is present in a large amount penetrates into water and becomes easily crystallized. As a result, since the fibers are elongated in the winding, they are elongated in the package, and the yarn layer is separated and broken at the time of winding and packaging, and it is difficult to stably wind up. Further, in the fiber-based fiber structure in which the elongation is excessively large, the amorphous portion is increased. When the yarn is taken up, the amorphous portion which is present in a large amount penetrates into the water and becomes easily crystallized. Since the fiber is stretched after being taken up, the yarn layer is separated and broken when the package is taken up, and it is difficult to stably wind up. Further, the final product of the fiber having an excessive elongation is lowered in the cleaning fastness. Taking these problems into consideration, the optimum elongation is set to 70 to 150%, and more preferably 80 to 150%.

The polyamide fiber of the present invention preferably has a strength of 3.5 cN/dtex. the above. The quality of the final product or the yarn making effect is obtained by increasing the strength. When the strength is small, the high passability of the yarn processing, weaving, and knitting is deteriorated, and it is difficult to obtain the durability of the final product. More preferably, the strength is 4.0 cN/dtex or more.

The total fineness of the polyamide fiber of the present invention is suitable depending on the application. Local setting, but preferably 10~230dtex, and more preferably 10~200dtex. Further, the single fiber fineness can be appropriately set depending on the application, but it is preferably 0.5 to 10 dtex, and more preferably 0.5 to 5 dtex, in terms of softness during fabric processing.

The polyamide fiber of the present invention can be produced by a general spinning method as a basic spinning method, and the production process is not particularly limited on the premise that the polyamide fiber of the present invention can be obtained. Among them, it can be manufactured by the following manufacturing method.

The method is to melt the polyamidamine from the nozzle and become a yarn. In the strip, the sliver is cooled and solidified by cooling air, and after the sliver is attached to the spinning oil agent, the sliver is recovered and the sliver is further wound.

This method is more specifically described using FIG. Further, Fig. 2 is a conceptual diagram showing an example of a manufacturing process of the fiber of the present invention.

The molten polyamine is metered and pushed out by the gear pump 1, and is discharged from the spinning nozzle 2, and the polyamide is made into a fibrous yarn. The cooling air is blown by a cooling device 3 such as a chimney, and the sliver is cooled to near room temperature and the polyamide gauze is solidified. The yarn feeder is supplied with oil by the oil supply device 4 and simultaneously aggregated into a bundle. Further, the yarns are staggered by the staggered nozzle device 5, recovered by the first godet roller 6, and passed through the second godet roller 7, and then taken up by the winding device 8.

In the method for producing a polyamide fiber according to the present invention, the distance from the nozzle outlet to the oil agent for spinning is preferably 500 mm or more and 1500 mm or less. More preferably, it is 500 mm or more and 1200 mm or less, and more preferably 500 mm or more and 1000 mm or less. When the distance is short, there is a possibility that the oil is adhered before the end of the stretching and stretching, and the strong elongation of the obtained fiber is lowered. If the distance is large, shrinkage occurs due to excessive drafting during winding, and tension is generated after the winding, and the original yarn drum cannot be pulled, so that it tends to be difficult to produce stably.

The polyamine used in the polyamide fiber of the present invention has a water absorption ratio lower than that of the general polyamine 6 by 1.8% in terms of the ratio of the number of decyl groups to the number of methylene groups. In the case of the general polyamine 6 before the oil supply device 4 is supplied with oil, the glass transition temperature becomes lower than room temperature due to moisture absorption, and since the polymer chain is freely moved, even if the sliver is in the air The increase in the movement tension is also small. Further, the glass transition temperature of the polyamide yarn of the present invention is lower than that of the polyamide 6 and the glass transition point is usually 25 ° C or more at room temperature at the time of manufacture. Above the glass transition temperature, the polymer chain in the fiber does not move, and the tension generated by the movement of the yarn in the air increases. Therefore, even if the distance from the spinning nozzle 2 to the oil supply device 4 to which the spinning oil agent is attached is equal, the tension of the yarn of the polyamide fiber of the present invention is large. As a result, as the tension is increased, the stretching accompanying the air flow is increased until the first godet roller 6 is increased, and shrinkage occurs after being wound around the drum, which tends to be difficult to stabilize production due to the occurrence of the tension. . Therefore, the distance from the spinning nozzle 2 to the oil supply device 4 to which the spinning oil agent is attached is shortened, and the increase in the tension at the glass transition temperature or higher is reduced, whereby the polyamide fiber of the present invention can be obtained. Further, since the polyamine of the present invention, for example, polyamine 610 has a Young's modulus higher than that of polyamide 6, it is discharged from the spinning nozzle 2 until the oil is adhered thereto. The tension between the slivers tends to become larger. As described above, since the stretching to be added to the first godet roller 6 is an element of advancement, in order to obtain the polyamide fiber, it is desirable to supply the oiling device from the spinning nozzle 2 to the spinning oil agent. The distance until 4 is shortened.

For the above reasons, the exit of the spinning nozzle is attached The distance from the spinning oil agent is preferably 500 mm or more and 1200 mm or less, and more preferably 500 mm or more and 1000 mm or less.

Further, the spinning oil agent supplied by the oil supply device 4 is preferably. It is an aqueous oil agent. When the water-containing oil agent is applied, the moisture contained in the oil agent is generated in the middle of the yarn making process, and the glass transition point temperature of the polyamide is produced. The yarn tension between the self-priming device 4 and the staggered nozzle device 5 is reduced, and the stretching between the self-priming device 4 and the staggered nozzle device 5 can be suppressed, and the tightening is reduced.

Further, in the method for producing a polyamide fiber of the present invention, The recovery rate is preferably in the range of 3,300 m/min or more and 4,300 m/min or less. Further, the winding speed is preferably 0.8 to 1.2 times the recovery speed. In the manufacturing method shown in Fig. 2, the recovery speed means the peripheral speed of the first godet roller 6. The take-up speed is the peripheral speed of the take-up device 8.

Recovery rate, and the rate of recovery divided by the speed of the take-up speed It is the total amount of stretch that is used as an indicator of the orientation of the polymer, and can be stably produced within the range. If the total amount of stretching is too small, that is, the recovery speed is small, and the value of the recovery speed and the coiling speed is more than 1.2 times, the orientation of the fiber crystals is low, and the spinning oil or the moisture in the air is excessively absorbed, resulting in The sliver is swollen and cannot be stabilized. Further, when the total stretching amount is too large, that is, the recovery speed (circumferential speed of the first godet roller 6) exceeds 4,300 / minute, or the value of the recovery speed divided by the winding speed is less than 0.8 times, the fiber alignment cannot be performed, and the yarn is tight. Pulling can not stabilize production. The recovery rate is preferably in the range of 3,300 m/min or more and 4000 m/min or less, and the coiling speed is in the range of 0.8 to 1.2 times the recovery speed. More preferably, the recovery rate is in the range of 3,300 m/min or more and 3,800 m/min or less, and the winding speed is in the range of 1.0 to 1.2 times the recovery speed.

By setting the oil supply position, recovery speed, and take-up speed The above range can be stably produced without the occurrence of swelling and tight pulling in the spinning, and a good flat cylindrical package can be obtained.

Flat cylindrical package composed of the polyamide fiber of the present invention Preferably, the bulge is 10% or less. The expansion ratio indicates the degree of expansion of the end face of the package. As shown in Fig. 3, the width WB (mm) of the package is measured, and the width of the package WS (mm) at the beginning of the package is measured as {(WB-WS)/WS}. ×100 calculated value. Fig. 3 is a side cross-sectional view schematically showing the package of the flat cylindrical package of the present invention, showing a state in which the paper tube A is wound up by the yarn B.

If the expansion ratio exceeds 10%, then in the bale box or palette In the meantime, there is a problem in that it is difficult to carry out the wrapping at a predetermined place due to the expansion of the end surface of the package. Moreover, even if it can be bundled, the friction between the end face of the package and the bale material during conveyance causes scratching of the sliver (twisting of the monofilament, cutting of the monofilament), or causing the reelability of the sliver. Bad problem. More preferably, it is 8% or less.

Flat tube package composed of the polyamide fiber of the present invention The loading, especially when the amount of fibers on the packaging roll is 3 kg or more, is effective, especially when it is 4.5 kg or more. There is also no upper limit, but it is usually 7.5kg or less.

The polyamide fiber of the present invention can be used alone as it is It is preferably used on a fabric for use as a processing yarn for use on a fabric. The processing yarn is, for example, a false twisted textured yarn that imparts curling properties, and further has a stretched false twisted yarn and a fused false twisted yarn that express a rough portion and a thin portion of the texture. Further, a composite yarn having a structural characteristic of a woven fabric, which has a yarn length difference by blending a polyamide yarn of the present invention with a low elongation fiber yarn, may be mentioned. In the above composite yarn, the low elongation fiber yarn preferably has an elongation of less than 70%, more preferably 30 to 50%. Further, in the composite processing of the composite processed yarn of the present invention and the composite yarn of the one or more yarns and the composite false twist yarn, the same raw materials may be combined or different raw materials may be combined. Moreover, the manufacturing method can be processed simultaneously, or can be processed separately after processing.

As the polyamine fiber and the polyamidamine fiber using the present invention The fiber structure of the processed yarn (usually cloth) can be used for sportswear, pants, jackets, men's, women's clothing, women's short underwear, shorts and other close-fitting clothing such as shirts or jackets. Clothing, such as socks and socks, are used for clothing. It can also be used for raw materials used for clothing such as underwear cups or mats. It can also be used for indoor applications such as curtains or carpets, mats, furniture, and other industrial materials.

[Examples]

The invention will be described in detail by way of examples. Further, the measurement methods in the examples were as follows.

[test methods]

A. Relative viscosity of sulfuric acid

0.25 g of the sample was dissolved in 1 g of 100 ml of sulfuric acid having a concentration of 98% by mass, and the flow time (T1) at 25 ° C was measured using an Ostwald type viscometer. Next, the down time (T2) of sulfuric acid having a concentration of only 98% by mass was measured. The ratio of T1 to T2, that is, T1/T2 is set to the relative viscosity of sulfuric acid.

B. Intrinsic viscosity [IV]

0.8 g of the sample polymer was dissolved in 10 ml of orthochlorophenol (hereinafter abbreviated as OCP), and an Oswald type viscometer was used at 25 ° C to calculate the relative viscosity [ηr] by the following formula (IV). ).

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

Intrinsic viscosity [IV]=0.0242ηr+0.2634

Where η: viscosity of the polymer solution, η ₀ : viscosity of OCP, t: time of solution drop (seconds), q: density of solution (g/cm ³ ), t ₀ : drop time of OCP (seconds), q ₀ : density of OCP (g/cm ³ ).

C. Melting point (Tm)

Using a differential scanning calorimeter model DSC-7 manufactured by PerkinElmer Co., Ltd., 20 mg of a sample polymer was taken. As the first scan, the temperature was raised from 20 ° C to 270 ° C at a temperature increase rate of 20 ° C / min and held at a temperature of 270 ° C for 5 minutes. Thereafter, the temperature was lowered from 270 ° C to 20 ° C at a cooling rate of 20 ° C / min. After holding at 20 ° C for 1 minute, the second scanning was carried out, and the temperature was raised from 20 ° C to 270 ° C at 20 ° C / min. The temperature of the endothermic peak observed at this time was taken as the melting point.

D. Denier

The sample was made into a 200-wound skein using a cloth inspection machine with a frame circumference of 1.125 m, and dried using a hot air dryer (105 ± 2 ° C × 60 minutes), and the mass of the skein was measured with a balance (nominal moisture rate +1) The multiplier is obtained by multiplying the obtained value. Further, the specific moisture content was set to 4.5% for polyamine 6, polystyrene 610 to 2.5%, polyamine 510 to 3.0%, and polyamine 12 to 1.2%. The measurement system was carried out 4 times and the average value was set to the fineness. Further, the value obtained by dividing the obtained fineness by the number of filaments was defined as the single fiber fineness.

E. Strength and elongation

The sample was measured using the "TENSILON (trademark)" UCT-100 manufactured by Orientec Co., Ltd. under the constant elongation conditions shown in JIS L1013 (Chemical Fiber Yarn Test Method, 2010). set. The elongation is determined by the elongation at the point indicating the maximum strength in the tensile strength-elongation curve. Further, the strength is defined as the intensity by dividing the maximum strength by the value of the fineness. The measurement system was carried out 10 times and the average value was set as the strength and elongation.

F. boiling water shrinkage

The obtained polyamide fiber was wound 20 times with a skeining machine having a circumference of 1.125 m, and an initial length L ₀ was obtained under a load of 0.09 cN/dtex. Then, it was treated in boiling water under no load for 30 minutes and then air-dried. Next, the length L ₁ after the treatment was obtained under a load of 0.09 cN/dtex, and was calculated by the following formula.

Boiling water shrinkage rate (%) = [(L _{0 -} L ₁ ) / L ₀ ] × 100

G. Thickness of the tube knit material

Five subjects were compared and evaluated based on the following evaluation criteria for the thickness of the knitted material. Further, the comparison object was the sample of Comparative Example 8.

Excellent: very texture thickness

Good: There is a sense of texture thickness

Ordinary: no texture thickness sense (same as in Comparative Example 8)

Poor: no texture thickness (as compared to Comparative Example 8)

H. Full packaging rate

The full packaging rate obtained at the time of one ton of spinning was calculated by the following formula.

Full packaging rate (%) = [D ₁ / D ₀ ] × 100

D ₀ : theoretically the largest number of packages at the time of 1 ton of spinning

D ₁ : The actual number of packages obtained at the time of 1 ton of spinning

(Example 1)

Using polyamide 610 (sulfuric acid relative viscosity: 2.67, melting point: 225 ° C), the spun yarn was continuously applied to the spinning apparatus shown in Fig. 2 to obtain a polyamide fiber. The steps are as follows. First, the polyamide 610 was put into a spinning machine, melted at a spinning temperature of 270 ° C, and a polymer (35.7 g/min) was metered in a gear pump 1 and discharged, and introduced into a spinning nozzle 2 heated to 270 ° C. The surface of the spinning nozzle 2 having a hole having a hole diameter of 0.20 mm and a hole length of 0.5 mm was spun to obtain a sliver. The single-flow type cooling device 3 cools the sliver with air and solidifies it, and supplies oil to the oil supply device 4. Further, the oil supply device is disposed at a position of 800 mm from the surface of the spinning nozzle. The staggered nozzle device 5 was staggered, and the peripheral speed of the first godet roller 6 (i.e., the recovery speed) was recovered at 4094 m/min, and the peripheral speed of the second godet roller was set at 4094 m/min. The draw ratio was set to 1.0. Further, the take-up speed was taken up at 4000 m/min to obtain a 6 kg flat cylindrical package composed of 96 dtex (decitex) 68-filament nylon 610 fibers. In the spinning, there is no swell of the take-up reel and no tension is generated and it is extremely stable and can be produced. Further, most of them are produced in a flat cylindrical package, and as a result, the full packaging rate is 100%. The results of the obtained fibers are shown in Table 1.

(Example 2)

A flat cylindrical package of 6 kg of multifilament yarn 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 surface of the spinning nozzle. It can be produced without any swelling and tension in the spinning and is extremely stable. The full packaging rate is 95%. The results of the obtained fibers are shown in Table 1.

(Example 3)

A flat cylindrical package of 6 kg of multifilament yarn 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 surface of the spinning nozzle. It can be produced without any swelling and tension in the spinning and is extremely stable. The full packaging rate is 90%. The results of the obtained fibers are shown in Table 1.

(Example 4)

The peripheral speed of the first godet roller 6 was set to 4264 m/min, the peripheral speed of the second godet roller 7 was set to 4264 m/min, the draw ratio was set to 1.0, and the take-up speed was set to 4200 m/min. Further, a flat cylindrical package of 6 kg of multifilament yarn was obtained under the same conditions as in Example 1. It can be produced without any swelling and tension in the spinning and is extremely stable. The full packaging rate is 100%. The results of the obtained fibers are shown in Table 1.

(Example 5)

The peripheral speed of the first godet roller 6 was set to 3,839 m/min, the peripheral speed of the second godet roller 7 was set to 3,839 m/min, the draw ratio was set to 1.0, and the take-up speed was set to 3,800 m/min. Further, a flat cylindrical package of 6 kg of multifilament yarn was obtained under the same conditions as in Example 1. It can be produced without any swelling and tension in the spinning and is extremely stable. The full packaging rate is 100%. The results of the obtained fibers are shown in Table 1.

(Example 6)

The peripheral speed of the first godet roller 6 was set to 3722 m/min, the peripheral speed of the second godet roller 7 was 4094 m/min, the draw ratio was 1.1, and the take-up speed was 4000 m/min. Further, a flat cylindrical package of 6 kg of multifilament yarn was obtained under the same conditions as in Example 1. It can be produced without any swelling and tension in the spinning and is extremely stable. The full packaging rate is 95%. The results of the obtained fibers are shown in Table 1.

(Example 7)

The peripheral speed of the first godet roller 6 was set to 3,321 m/min, the peripheral speed of the second godet roller 7 was set to 3,819 m/min, the draw ratio was set to 1.15, and the take-up speed was set to 3,800 m/min. Further, a flat cylindrical package of 6 kg of multifilament yarn was obtained under the same conditions as in Example 1. It can be produced without any swelling and tension in the spinning and is extremely stable. The full packaging rate is 95%. The results of the obtained fibers are shown in Table 2.

(Example 8)

The peripheral speed of the first godet roller 6 was set to 3,327 m/min, the peripheral speed of the second godet roller 7 was set to 3,660 m/min, the draw ratio was set to 1.05, and the take-up speed was set to 3,600 m/min. Further, a flat cylindrical package of 6 kg of multifilament yarn was obtained under the same conditions as in Example 1. It can be produced without any swelling and tension in the spinning and is extremely stable. The full packaging rate is 95%. The results of the obtained fibers are shown in Table 2.

(Example 9)

The polymer (23.6 g/min) was metered using a gear pump 1 and spun from a spinning nozzle 2 having a circular hole having a 24-hole discharge opening diameter of 0.30 mm and a hole length of 0.75 mm, except that it was the same as in Example 1. Under the conditions of the conditions, a flat cylindrical package of 6 d's total fineness of 64 dtex and 24 filaments of multifilament 6 kg was obtained. It can be produced without any swelling and tension in the spinning and is extremely stable. The full packaging rate is 100%. The results of the obtained fibers are shown in Table 2.

(Embodiment 10)

Self-contained 20-hole discharge aperture 0.20mm, hole length 0.50mm The spinning nozzle 2 of the circular hole was spun, and the oil supply device was placed at a position of 1500 mm from the nozzle surface, and a multifilament of 96 dtex and 20 filaments was obtained under the same conditions as in Example 1. 6kg flat cylindrical packaging. It can be produced without any swelling and tension in the spinning and is extremely stable. The full packaging rate is 90%. The results of the obtained fibers are shown in Table 2.

(Example 11)

The polymer was metered using a gear pump 1 (16.2 g/min) In the same manner as in Example 1, except that the spinning nozzle 2 which spouted a circular hole having a hole diameter of 0.20 mm and a hole length of 0.50 mm was spun, the total fineness of the two packages was 44 dtex and 34 filaments. Multi-filament 6kg flat cylindrical packaging. It can be produced without any swelling and tension in the spinning and is extremely stable. Also, the full packaging rate is 100%. The results of the obtained fibers are shown in Table 2.

(Embodiment 12)

Polyamide 12 (sulfuric acid relative viscosity 2.20, melting point: 180 ° C), the spinning nozzle was melted at a temperature of 250 ° C, and the spinning nozzle 2 heated to 250 ° C was introduced, and a flat cylindrical package of 6 kg of multifilament was obtained under the same conditions as in Example 1. It can be produced without any swelling and tension in the spinning and is extremely stable. The full packaging rate is 100%. The results of the obtained fibers are shown in Table 2.

(Example 13)

Polyacetamide 510 with a relative viscosity of 2.62 (melting point: A flat cylindrical package of 6 kg of multifilament yarn was obtained under the same conditions as in Example 1 except that the spinning nozzle 2 heated to 250 ° C was introduced at 216 ° C. No swelling and no tension in the spinning and extreme It is stable and can be produced. The full packaging rate is 100%. The results of the obtained fibers are shown in Table 2.

(Comparative Example 1)

In the same manner as in the first embodiment, the position of the oil feeding device was set to 1800 mm from the surface of the spinning nozzle, and the tension was pulled at the time of winding, and the package could not be taken out from the winding device. Therefore, as a result, the flat cylindrical package of the multifilament cannot be obtained, and the production cannot be stabilized.

(Comparative Example 2)

In the same manner as in the first embodiment, the position of the oil supply device was set to be at a position of 300 mm from the surface of the spinning nozzle, and the oil was applied to the staggered nozzle device 5 at the time of trial winding. As a result, the tension of the sliver becomes low, and the tension of the yarn of the first godet 6 becomes good. Therefore, as a result, the flat cylindrical package of the multifilament cannot be obtained, and the production cannot be stabilized.

(Comparative Example 3)

The peripheral speed of the first godet roller 6 was set to 4592 m/min, the peripheral speed of the second godet roller 7 was set to 4592 m/min, the draw ratio was set to 1.0, and the take-up speed was set to 4500 m/min. Further, a multifilament or flat cylindrical package was obtained under the same conditions as in Example 1. In spinning, tension is frequently generated. The self-winding device can obtain the package and obtain a flat cylindrical package of 6kg multifilament. As a result, the full packaging rate was 40%, and it was impossible to stabilize production. Further, the obtained multifilament had an elongation of 63% and a strength of 4.9 cN/dtex, and no high elongation was observed. Further, the obtained flat cylindrical package had an expansion ratio of 12.0%, and could not be fixed to a predetermined place of a carton or a palette and was bundled.

(Comparative Example 4)

The peripheral speed of the first godet roller 6 was set to 3108 m/min. In the same manner as in Example 1, except that the peripheral speed of the second godet roller 7 was 4040 m/min, the draw ratio was 1.3, and the take-up speed was 4000 m/min. . In spinning, tension is frequently generated. The self-winding device can obtain the package and obtain a flat cylindrical package of 6kg multifilament. As a result, the full packaging rate was 50%, and it was impossible to stabilize production. Further, the obtained fiber had an elongation of 60% and a strength of 5.2 cN/dtex, and no high elongation was observed. Further, the obtained flat cylindrical package had an expansion ratio of 12.5%, and could not be fixed to a predetermined place in a carton or a palette and was bundled.

(Comparative Example 5)

Polyamide 6 (sulfuric acid relative viscosity 2.62, melting point: 220) In the same manner as in Example 1, except that the temperature was °C, the methylene number was 1:5), and as a result, the fiber swelling due to moisture absorption at the time of winding was caused, and wrinkles of the yarn layer of the take-up package were caused. , failed to obtain multifilament, flat cylindrical packaging, and can not be stable production.

Comparing Examples 1 to 13 described in Tables 1 and 2 with the above comparison As a result of the examples 1 to 5, according to the invention of the method for producing a polyamide fiber, it is possible to produce the product stably without being swollen and tightly stretched in the spinning.

(Examples 14 to 16)

Polypropylene terephthalate having an intrinsic viscosity [IV] of 1.40 (poly trimethylene terephthalate) and polyethylene terephthalate having an intrinsic viscosity [IV] of 0.51 were melted at a spinning ratio of 275 ° C at a weight ratio of 50:50, introduced into a spinning container, and melted and discharged. After the spouted gauze is cooled, it is recovered at 1200 m/min in a recovery roll heated to 55 ° C to 4200 m/min was pulled back, stretched, heat treated at a stretching roll heated to 155 ° C, and then subjected to fluid interlacing treatment using an interlacing device. Thereafter, it was recovered at a stretching ratio of -4.5% (speed: 4011 m/min) using a non-heated third roll, and recovered at 4011 m/min using a non-heated fourth roll, and then taken up by a coiler to obtain 33 dtex12 silk polyester composite multifilament composed of flat cylindrical packaging.

The 96 dtex 68 silk polyamidamine 610 multifilaments obtained in Example 1, Example 5, and Example 9 were prepared as sheath yarns, respectively. A polyester-based composite multifilament (denier 33 dtex, elongation 34%, strength 3.7 cN/dtex) of a flat cylindrical package 33 shown above was prepared as a core yarn. Using the composite false twisting machine shown in Fig. 4 (manufactured by Aiko Seisakusho Co., Ltd.), the sheath yarn and the core yarn were used for the composite processing to obtain a composite processed yarn of 129 dtex and 88 filaments.

This specific method will be described with reference to FIG. First, the sheath yarn is supplied from the sheath package 10 via the sheath yarn feed roller 11. This yarn is heated by the false twist heater 13 while being twisted by the squeegee 12, and the sheath yarn is collected by the recovery roller 15 for the sheath yarn, and is supplied to the nozzle 16. On the other hand, the polyamide fiber is recovered from the core yarn package 9 by the core yarn recovery roller 14 and supplied to the nozzle 16. The sheath yarns and the core yarns supplied to the nozzles 16 are interlaced by the nozzles 16. The interlaced yarns are set as processed yarns, and are taken up to the take-up device 18 via the recovery rolls 17. The composite processed yarn 19 is obtained.

Further, the processing conditions were a processing speed of 250 m/min, a false twist ratio of 1.22 times, a heater temperature of 190 ° C, a D/Y ratio of 1.6 times, and a twister set to a three-axis type.

If the composite processed yarn is observed, the polyester portion of the core is formed. The position of the multifilament yarn relative to the central portion of the composite processed yarn, the polyamide 610 multifilament system forming the sheath portion has a yarn length difference with respect to the polyester composite multifilament yarn. The composite processed yarn was placed in a flat state in a free state, and the difference in length of the yarn was observed. When the yarns of Example 7, Example 5, and Example 1 were compared, the yarn length difference of Example 7 was the highest, and Example 1 was the lowest. When the obtained composite processed yarn is produced into a tubular knitted fabric and the woven fabric structure is evaluated, the texture thickness is increased as the yarn length difference is increased. The results are shown in Table 3.

(Examples 17 to 18)

The 96 dtex 68 silk polyamine obtained in Example 12 A composite yarn of 129 dtex and 88 filaments was obtained by the same procedure as in Example 14 except that the multifilament yarn of the multifilament yarn of the 96 dtex and 68 filaments obtained in Example 13 was used as a sheath yarn. A tubular knitted fabric was produced in the same manner as in Example 14 of the obtained composite processed yarn. The evaluation is shown in Table 3.

(Comparative Example 7)

96dtex68 silk polyamine obtained in Comparative Example 4 The 610 multifilament yarn was used as a sheath yarn, and composite processing was carried out in the same manner as in Example 14 to obtain a composite processed yarn of 129 dtex and 88 filaments. A tubular knitted fabric was produced in the same manner as in Example 14 of the obtained composite processed yarn. The evaluation is shown in Table 3.

(Comparative Example 8)

Polyamide 6 (sulfuric acid relative viscosity 2.62, melting point: 220) °C, methylene number 1:5), recovered at a peripheral speed of the first godet roller 6 at 4545 m/min, the peripheral speed of the second godet roller 7 was 4545 m/min, and the draw ratio was 1.0, at a take-up speed. Winding at 4500m/min, get 96dtex68 silk polyamine 6 multifilament. Further, the fineness was 96.0 dtex, the elongation was 60%, and the strength was 4.5 cN/dtex.

The obtained 96 dtex 68-filament polyisamine 6 multifilament was used as a sheath yarn, and composite processing was carried out in the same manner as in Example 14 to obtain a composite processed yarn of 129 dtex and 88 filaments. A tubular knitted fabric was produced in the same manner as in Example 14 of the obtained composite processed yarn. The evaluation is shown in Table 3.

As is apparent from the results of Table 3, by using the polyamide fiber of the present invention, a knitted fabric having a good texture and a good texture can be obtained.

Claims (7)

A polyamidamine fiber which is a polydecylamine having a polymer of the structural formula A shown below, or a polyamidoamine of a polymer of the structural formula B, having a structure of 90 mol% or more in the total guanamine unit a unit represented by Formula A or a unit represented by Structural Formula B, and having a strength of 3.5 cN/dtex or more and an elongation of 75 to 150%; The structural formula A is a structure having any value of 9 to 12, and the structural formula B is a structure having m and n of (m+n)/2 being any value of 6 to 12. The polyamide fiber of claim 1, wherein the polyamine is a polymer of structural formula B. The polyamine fiber of claim 1, wherein the polyamine is a polymer of structural formula A. A cheese-shaped package comprising the polyamine fiber of any one of claims 1 to 3, and having a bulge of 10% as shown by the following formula (I) the following B(%)={(WB-WS)/WS}×100......(I) (where B is the expansion ratio, WB is the maximum width of the package (mm), and WS is the width at which the package starts to be rolled up. (mm)). A method for producing a polyamide fiber, which is a method for producing a polyamide fiber according to any one of claims 1 to 3, which is characterized in that the molten polyamine is supplied from a nozzle. Discharged into a sliver, the gauze is cooled and solidified by cooling air, and after the sliver adheres to the spinning oil agent, the sliver is recovered and the sliver is further wound; (a) from the nozzle outlet to the spun yarn The distance from the oil agent is 500 mm or more and 1500 mm or less. (b) The recovery rate is 3300 m/min or more and 4300 m/min or less, and the winding speed is 0.8 to 1.2 times the recovery speed. A composite processed yarn comprising the polyamide fibers of any one of claims 1 to 3 and fibers having an elongation of less than 70%. A fabric comprising the polyamide fiber of any one of claims 1 to 3.