JP2000239960A - Heat-aging of polyurethane elastic fiber and wound yarn body - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a wound yarn body excellent in homogeneity of inner and outer layers and free from occurrence of density unevenness and warp streak, etc., even when dyed at high temperature by winding a polyurethane elastic yarn obtained by melt-spinning method around a core body in which at least the surface is constituted of Al and subjecting the yarn wound body to heat- aging treatment under specific conditions. SOLUTION: A polyurethane elastic yarn obtained by melt-spinning method is wound around a core body in which at least surface is constituted of Al and water content of the resultant yarn wound body is adjusted to <=2,000 ppm and the yarn wound body is subjected to heat aging treatment in a gas kept at 50-100 deg.C, preferably 60-95 deg.C at -20 deg.C to +25 deg.C dew point, preferably for 3-36 hr in order to carry out solid phase polymerization and crystallization of hard segment to provide the objective wound yarn body in which residual strain after hot water treatment of innermost layer of the above wound yarn body is <=67% and relative viscosity difference of fibers between innermost layer part and outermost layer part is 0.01-0.03.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a method for heating and aging polyurethane fibers, a method for dyeing polyurethane fibers, and a wound body.

[0002]

2. Description of the Related Art Dry spinning, wet spinning, and melt spinning are known as methods for producing polyurethane elastic fibers. Among them, polyurethane elastic fibers obtained by melt spinning can be finely deniered. In addition, attention is paid to its transparency, good transparency, and low cost. However, the polyurethane elastic fiber obtained by the melt spinning method is hard to generate strong hard segments because the thermoplastic polyurethane is once melted, and is lower in temperature than the fiber obtained by the dry spinning method and the wet spinning method. There is a tendency that heat resistance such as recoverability and resistance, and hot water resistance are inferior.

Various proposals have been made to solve the above problems. For example, a polyurethane elastic fiber is wound after melt-spinning, and the resulting wound body is heat-treated at a temperature of 60 to 150 ° C. for about 1 to 48 hours ( Heat aging treatment) to perform solid-phase polymerization and hard segment crystallization has been proposed.

[0004]

However, when the wound body is subjected to a heat aging treatment, the heat resistance of the outermost layer of the wound body is greatly improved, but the heat resistance of the innermost layer is lower than that of the outermost layer. Various problems have arisen because they are not improved as compared with the conventional art. That is, when a fibrous structure such as a fabric is manufactured, a portion having a low heat resistance and a low hot water resistance (a portion where the fiber constituting the innermost layer of the wound body is present) is formed. -Even if the hot water resistance is excellent, it cannot be satisfactory as a fiber structure. In particular, when cross-woven with another fiber such as nylon or polyester and subjected to high-temperature dyeing or high-temperature high-pressure dyeing, unevenness in density or warping occurs due to the presence of a portion having low heat resistance and hot water resistance. It is an object of the present invention to provide a heat-aging method for obtaining a wound body having high heat resistance and hot water resistance in the innermost layer and excellent homogeneity in the same cheese, and a wound body excellent in various properties. Another object of the present invention is to provide a high-temperature dyeing method that does not cause uneven density or warping of polyurethane elastic fibers or a fiber structure containing the polyurethane elastic fibers.

[0005]

SUMMARY OF THE INVENTION The present invention relates to (1) a method of heating and aging a wound yarn obtained by winding a polyurethane elastic fiber obtained by a melt spinning method on a core having at least a surface made of aluminum. A method of heating and aging polyurethane elastic fibers to be subjected to the treatment, (2) a dew point of −20 ° C. on a wound body obtained by winding the polyurethane elastic fibers obtained by the melt spinning method on a core body having at least a surface made of aluminum; (3) a method of heating and aging polyurethane elastic fibers in a gas at a temperature of 50 to 100 ° C. and a temperature of 50 to 100 ° C., (3) a core body in which the polyurethane elastic fibers obtained by melt spinning have at least a surface made of aluminum Elastic fiber obtained by subjecting a wound body wound to a roll to a heat aging treatment or a fiber containing the polyurethane elastic fiber Method of applying a high temperature dyeing the concrete body,
(4) A polyurethane elastic fiber wound wound around a core body after being spun by a melt spinning method, wherein the innermost layer of the wound body has a residual strain of 68% or less after heat-resistant water treatment. Thread (5) The difference in relative viscosity of the fibers between the innermost layer portion and the outermost layer portion of the wound body is 0.01 to -0.03 (4).
And a wound polyurethane elastic fiber wound body.

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, a specific bobbin is used to suppress the transfer of water from the bobbin to the innermost layer of the cheese during the heat aging treatment, and at the same time, the temperature of the inner layer is controlled by the temperature of the heat aging treatment atmosphere. By maintaining the temperature in the vicinity, the heat resistance and the hot water resistance of the innermost layer are increased to improve the homogeneity. When the polyurethane is melted, a part of the polyurethane is dissociated into NCO groups and OH groups, so that the polyurethane produced by the melt spinning method necessarily contains NCO groups. Next, after spinning, a recombination reaction in a dissociated state proceeds, and the yarn quality and thermal properties change over time.

[0007] In addition to performing solid phase polymerization, crystallization of the hard segment is advanced, and a heat aging treatment is performed to complete such a reaction.
Hot water resistance and the like are improved. That is, when the dissociated NCO group reacts with alcohol, water, etc. to form a urethane bond or a urea bond, and further, the dissociated NCO group forms a primary structure such as an allohanate bond, a burette bond by a reaction with the urethane bond or the urea bond. At the same time, a higher-order structure such as microphase separation property and hard segment cohesion property of polyurethane is formed.

When the wound body is subjected to a heat aging treatment, solid phase polymerization and crystallization of hard segments proceed first in the outermost layer portion of the wound body, and then the same reaction occurs in the innermost layer portion of the wound body as the temperature rises. However, if the core contains water at this time, the water present in the core is transferred to the innermost layer of the wound thread as needed. Further, there is a problem that the temperature of the innermost layer of the wound body tends to be lower than that of the outermost layer. For this reason, solid-state polymerization and crystallization of hard segments proceed efficiently in the outermost layer, but in the innermost layer, many of the dissociated NCO groups react with water due to the presence of excess water, causing chain elongation. As a result, the reaction between the dissociated NCO groups and the urethane bonds does not proceed sufficiently and the microseparability of polyurethane and the progress of aggregation of the hard segments are hindered, and the aging treatment is performed because the temperature is lower than that of the outermost layer. There was a problem that was difficult to progress. As a result, even when the heat aging treatment is performed, the heat resistance and the hot water resistance are not improved in the innermost layer portion of the wound body as compared with the outermost layer portion, and the performance as the whole wound body is lowered, and the homogeneity is further insufficient. Therefore, for example, when high-temperature dyeing is performed, spots are generated. Generally, a paper tube whose surface is covered with cellophane is used as the core of the wound body, and the paper tube usually contains 6 to 8% of water. Such a problem will occur.

According to the present invention, at least the surface of the core is made of aluminum so that the solid phase polymerization and the hard segment crystallization can be efficiently performed even in the innermost layer of the wound body. Aluminum has excellent water vapor shielding properties, so that moisture in the core does not move to the innermost layer of the wound body, and because of its excellent thermal conductivity, heat is generated inside the wound body during heat aging. The ripening treatment can be carried out efficiently and uniformly, since the heat is easily transmitted and the local heating by radiation from the core to the wound body is less likely to occur due to the low thermal emissivity. In addition, aluminum is more lightweight and advantageous in terms of cost, so that it has a better effect.
The thickness of the aluminum may be set as appropriate, but may preferably be in terms of the water shielding effect becomes moisture permeability 0~0.5g / m ² / 24hr thick, and more preferably does not substantially transmitted through the water vapor .

The core used in the present invention only needs to have at least the surface made of aluminum. Of course, all of the core may be made of aluminum, but it is sufficient that at least the surface is made of aluminum from the viewpoint of obtaining the effects of the present invention. For example, by coating the surface of a paper tube with aluminum, a core suitable for the present invention can be obtained, and favorable results can be obtained in terms of lightness and cost. The composition and the like of the paper tube are not particularly limited, and for example, a paper tube made of kraft paper widely known in the art may be used.

At this time, the thickness of the aluminum layer on the surface of the core body is set to 0.001 to 0.2 mm, particularly 0.01 to 0.05 mm from the viewpoints of handleability, light weight, water shielding property, heat conductivity and the like.
It is preferred that The method of integrating the water-shielding substance is not particularly limited, and may be a thermocompression bonding or a coating and integrating with an adhesive or the like. From the viewpoint of thermal conductivity, it is preferable to provide one or more aluminum layers not only on the core body surface but also inside the core body. The thickness of the aluminum layer formed inside the core body is 0.00 from the viewpoint of handleability, light weight, water shielding property, heat conductivity and the like.
It is preferably from 1 to 0.2 mm, especially from 0.01 to 0.05 mm. It is not necessary that the entire surface of the core body is made of aluminum, but it is preferable that the winding portion with which the fiber comes into contact is made of at least aluminum. Preferably it is.

The form of the core is not particularly limited, and is not particularly limited as long as the fiber can be wound up. From the viewpoint that the fiber can be wound up uniformly, it is preferable that the fiber is cylindrical (tubular), particularly hollow cylindrical (tubular), and it is more preferable that the cross section is a perfect circle. The diameter of the tube may be determined as appropriate, but from the viewpoints of winding efficiency, heat aging efficiency and the like, the diameter is preferably 3 to 20 cm, particularly preferably about 5 to 15 cm, and the length is 1 to 20 cm, especially It is preferably 3 to 10 cm. When hollow, the thickness of the core is 1 to 10 m
m is preferable. From the same viewpoint, it is preferable that the thickness of the fiber layer in the wound body (the distance from the surface of the core body to the surface of the outermost layer of the wound body) is 1 to 5 cm, and the fiber winding width is 3 to 10 cm.

From the viewpoint of heat resistance and hot water resistance of the fiber, the residual strain of the innermost layer of the wound body after the hot water treatment is preferably 67% or less, particularly preferably 65% or less, and more preferably 63% or less. The residual strain of the outermost layer of the wound body after the hot water treatment is also 67% or less, preferably 65% or less, and more preferably 63% or less. From the viewpoint of enhancing the homogeneity of the fibers and suppressing the occurrence of spots when subjected to high-temperature dyeing, the residual strain difference after the above-mentioned hot water treatment is preferably 1% or less, particularly preferably substantially 0%. Further, the relative viscosity difference (Δη: relative viscosity of the fiber in the innermost layer−relative viscosity of the fiber in the outermost layer) of the innermost layer portion and the outermost layer portion of the wound body is 0.01 to −
It is preferably 0.03, particularly preferably 0.00 to -0.02. If the difference in residual strain or the difference in relative viscosity is small, it can be said that the reaction during heat aging and the aggregation state of the hard segments are uniform. Even with high pressure dyeing,
Density unevenness and warping due to the inhomogeneity of various physical properties of the polyurethane elastic fiber hardly occur, and the polyurethane elastic fiber has high quality and excellent practicability. The relative viscosity of the innermost layer and the innermost layer is 1.8.
It is preferably set to 2.0.

In the present invention, the innermost layer means a fiber layer portion closest to the core of the wound body, specifically 2 mm from the core.
The outermost layer portion is a portion within 2 mm from the outermost part of the wound body. In the examples, each measurement is performed except for a portion within 5 mm from both ends of the core body.

The polyurethane which can be applied to the present invention is not particularly limited, and a known thermoplastic polyurethane can be used. A thermoplastic polyurethane obtained by reacting a polymer polyol, an organic diisocyanate and a chain extender is preferably used. Can be used. As the polymer diol constituting the polyurethane, at least one of polyester polyol, polycarbonate polyol, and polyether polyol is used.
Seeds can be used. From the viewpoints of spinnability, heat resistance and hot water resistance of fibers, and elasticity, the average molecular weight is 1000 to 60.
00, especially 1000-5000. It is preferable to use a polyester polyol from the viewpoint of efficiently obtaining fiber performance and the effects of the present invention, and polyurethane may be polymerized using two or more kinds of polyester polyols.

The diol component constituting the polyester diol is not particularly limited, but includes 1,4-butanediol,
Linear diols such as 1,5-pentanediol, 1,6-hexanediol, 1,8-octanediol, 1,9-nonanediol; 2-methyl-1,3-propanediol, neopentyl glycol, 3-methyl1, Examples include branched diols such as 5-pentanediol and 2-methyl-1,8-octanediol; and alicyclic diols such as cyclohexanedimethanol. Glycerin, trimethylolpropane, butanetriol,
Polyfunctional polyols such as hexanetriol, trimethylolbutane, and pentaerythritol may be used in combination. It is preferable to use 3-methyl-1,5-pentanediol from the viewpoint of hot water resistance and heat resistance of the fiber.

The dicarboxylic acid constituting the polyester polyol is not particularly limited, but may be a linear dicarboxylic acid such as glutanic acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, decanedicarboxylic acid or the like. Ester-forming derivatives; terephthalic acid,
Examples thereof include aromatic dicarboxylic acids such as phthalic acid and naphthalenedicarboxylic acid isophthalate, and ester-forming derivatives thereof; alicyclic dicarboxylic acids such as cyclohexanedicarboxylic acid, and ester-forming derivatives thereof. Furthermore, a polycarboxylic acid such as trimellitic acid may be used in combination. From the viewpoint of fiber performance, it is preferable to use one or more dicarboxylic acids selected from adipic acid, azelaic acid, and sebacic acid.

Heat resistance of the obtained polyurethane elastic fiber,
From the viewpoint of hot water resistance, a diol component having 6 to 10 carbon atoms having a methyl branch, such as 3-methyl-1,5-pentanediol or 2-methyl-1,8-octanediol, as a diol component; It is preferable to use a mixture of linear diols having a carbon number of 4 such as azelaic acid, sebacic acid and adipic acid as the dicarboxylic acid component.
It is preferred to use from 10 to 10 dicarboxylic acids. Among them, it is preferable to use a polyurethane polyol obtained by using 3-methyl-1,5-pentanediol as a diol component and one or more dicarboxylic acids selected from adipic acid, azelaic acid, and sebacic acid as a dicarboxylic acid component. By using such a polyester polyol, a polyurethane having excellent hot water resistance and heat resistance can be obtained. However, by adopting the heat aging method of the present invention, higher performance can be obtained.

The organic diisocyanate used in the synthesis of the polyurethane is not particularly limited, but 4,4'-diphenylmethane diisocyanate, p-phenylene diisocyanate, toluylene diisocyanate, 1,5-
Diisocyanates having a molecular weight of 500 or less such as naphthylene diisocyanate, xylylene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, and 4,4'-dicyclohexylmethane diisocyanate can be suitably used. Above all, molecular weight 200-50
Organic isocyanates of 0 are preferred, especially 4,4 '.
-Diphenylmethane diisocyanate is preferred. In addition, a compound having a blocked isocyanate group which is converted into free isocyanate as the organic diisocyanate can also be used.

The chain extender that can be used is not particularly limited, but a low molecular weight compound having at least two hydrogen atoms capable of reacting with isocyanate, for example, a molecular weight of 40
0 or less ethylene glycol, propylene glycol,
1,4-butanediol, 1,4-bis (2-hydroxyethoxy) benzene, 1,6-hexanediol,
Diols such as -methyl-1,5-pentanediol; and diamines such as hydrazine and propylene diamine. These chain extenders may be used alone or in combination of two or more. In particular, it is preferable to use 1,4-butanediol and 1,4-bis (2-hydroxyethoxy) benzene in view of heat resistance and hot water resistance of the obtained polyurethane.

The composition ratio of each component of the polyurethane used to obtain the polyurethane elastic fiber of the present invention, for example, the polymer diol (A), the organic isocyanate (B), and the chain extender (C) is determined by the ratio of the fiber. In terms of heat resistance and hot water resistance, the molar ratio of (B) / [(A) + (C)] is 0.99 or more.
It is preferably 1.20, more preferably 1.00 to 1.15. Even when the polymerization is carried out at the composition ratio, a method of adding and mixing an isocyanate compound at the time of spinning to obtain the composition ratio as a result is suitably adopted. In order to improve the polymerization / spinning speed, the polymerization / spinning may be performed by adding a trace amount of a tin catalyst in which urethane has a reaction activity.

The method of melt-spinning polyurethane elastic fibers is not particularly limited, but from the viewpoint of efficiency and thermal stability, a method in which polyurethane is polymerized and then directly supplied to a spinning device and spun (polymerization direct spinning method). It is preferable to employ it. More specifically, it is continuously supplied to a twin-screw extruder to supply 240 to 2
Continuous melt polymerization is carried out at 60 ° C., and then this is directly supplied to a spinning machine equipped with a single-screw extruder to obtain a spinning temperature of 205 to 235.
° C, cooling air dew point 0 ~ 20 ° C, spinning speed 200 ~ 800m
A preferred method is a method of spinning under the condition of / min. At this time, the fiber may be spun using two or more kinds of polyurethane.

The wound body may be subjected to a heat aging treatment. However, from the viewpoint of promoting solid phase polymerization and hard segment crystallization more efficiently, not only aluminum is used for the core but also heat aging treatment. It is preferable to adjust the water content of the fiber to be provided. Specifically, fiber moisture content 2000ppm
Hereinafter, it is particularly preferable to be 1000 ppm or less, and more preferably 600 ppm or less. By adjusting the content of the fiber, the heat aging treatment is performed more efficiently, and an excellent effect is obtained. The method for reducing the water content of the fiber is not particularly limited, but a method in which the steps from spinning to heat aging are performed under low humidity, a method of dehydrating before heat aging, and a temperature as low as 30 to 70 ° C. before heat aging. And a method of performing a reduced pressure heat treatment method.

Although the specific method of the heat aging treatment is not particularly limited, it is preferable to control the dew point of the atmosphere gas from the viewpoint of efficiently performing the heat aging treatment and increasing the heat resistance and hot water resistance of the fiber. The temperature is preferably from -20 ° C to + 25 ° C, particularly preferably from -5 ° C to + 5 ° C. By reducing the amount of water in the heat treatment atmosphere, solid phase polymerization and crystallization of hard segments can be more efficiently promoted, and excellent effects can be obtained in combination with the use of aluminum for the core.
Further, from the viewpoint of efficiently performing the heat aging treatment, the temperature of the gas is preferably set to 50 to 100 ° C, particularly preferably 60 to 95 ° C, and the heat aging treatment time is set to 1 to 48 hours, particularly 3 to 36 hours. Is preferred. More preferably, after the heat aging treatment, the temperature is 3 to 40 ° C. and 30 to 70% relative humidity.
It is preferable that the fiber performance is further stabilized by leaving it for 10 to 10 days. The fineness of the fiber may be set according to the purpose,
From the viewpoints of handleability, mechanical performance, elasticity, etc., it is preferable to set it to about 1 to 50d.

The fiber constituting the wound body of the present invention can be used for all purposes because of its excellent homogeneity, heat resistance and hot water resistance, and is particularly suitable as a material for clothing. Although the fibers can be used as they are, they may be processed into fiber structures such as spun yarns, woven and knitted fabrics, and nonwoven fabrics. Above all, the knitted fabric has a remarkable effect because of its excellent elastic performance, and may be dyed after the fiber structure is formed as required. Further, since the fiber is excellent in heat resistance, hot water resistance, and homogeneity, even when subjected to high-temperature dyeing or high-temperature high-pressure dyeing, density unevenness, warping, and the like are hardly generated, and an excellent effect is obtained. Further, a fiber structure may be formed by using fibers other than the elastic fibers in combination, and for example, may be used in combination with polyester fibers or nylon fibers. Polyester fiber is dyed at high temperature and high pressure due to low dyeability, and conventionally high-temperature dyeing is applied to the fiber structure using both of them, because the hot water resistance and homogeneity of polyurethane fiber are low. Although it was difficult to obtain a product, good results are obtained according to the present invention. The dyeing method is not particularly limited, and for example, a conventionally known method may be employed. The high-temperature dyeing referred to in the present invention refers to dyeing which is performed under a temperature condition of 110 ° C. or more, particularly 120 ° C. or more, and further 125 ° C. or more. By performing such dyeing, a knitted fabric for clothing having excellent performances can be obtained.

[0026]

EXAMPLES The present invention will now be described specifically with reference to examples, but the present invention is not limited to these examples. In addition, each measured value in an Example was measured and evaluated by the following methods. Measured according to the moisture permeability ^{g / m 2 / 24hr] JIS} Z0208.

[Fiber moisture content ppm] Measured by Karl Fischer method. Next, the wound body of the fiber was placed in a closed container and dried under reduced pressure by a vacuum pump. Trap between vacuum pump and container (refrigerant: acetone and dry ice)
Were installed, and evaporated water and oil were collected. Thereafter, the water and the oil agent were taken out of the trap, only the water was separated, its weight was measured, and the amount of water remaining in the wound body was calculated from the water content immediately after spinning. In addition, it is necessary to confirm that the water content of all the sealed containers and equipment is small and does not affect the water content measurement of the wound body, and the water content of the core (bobbin etc.) may affect the fiber water content. In some cases, the measurement is performed by replacing the core with a moisture-free core (for example, a bobbin made of Bakerat).

[Relative Viscosity of Fiber] The polyurethane elastic fiber of each layer of the wound body was dissolved in N, N-dimethylformamide containing 1% by weight of n-butylamine at a concentration of 0.5 g / dl, and was dissolved at 20 ° C. for 24 hours. After stirring for an hour, the relative viscosity (η) was measured in a thermostat at 30 ° C. using an Ubbelohde viscometer.
r) = t / t0. Here, t is the number of seconds of drop measured for the sample solution, and t0 is the number of seconds of drop measured for N, N-dimethylformamide containing 1% by weight of n-butylamine as a solvent using the same Ubbelohde viscometer.

[Residual strain% after heat resistance test] An elastic fiber sample was fixed in a state of being stretched by 200% using a wooden frame or the like.
After a dry heat treatment at 140 ° C for 2 minutes,
The sample was treated with hot water at 0 ° C. for 30 minutes, the length of the sample immediately after the release of stress was measured, and the residual strain S was calculated according to the following equation. Residual strain S is a measure of the elongation of the sample after hot water treatment,
It can be said that the smaller the value is, the more excellent the hot water resistance is. L is the length of the sample after the hot water treatment, and L0 is the length of the sample before the hot water treatment. S = {(L−L0) / 2L0} × 100

[Evaluation of density unevenness after dyeing / inch, warping] Polyurethane elastic yarn of about 40 denier was drawn into polyester drawn yarn 50dr / 48f (bright, T-shaped yarn,
Knitted together with a crimp value K1 = 0) using a tricot machine, and then subjected to a dyeing finish process, and the average density (wale density, course / in) of the outermost layer and innermost layer of the finished polyurethane elastic fiber was measured. To evaluate the density unevenness. ◎ (extremely good) when no warp muscle was observed, ○ (good) when hardly warp was seen, △ (poor) when warp was slightly observed The cross muscle was evaluated as x (extremely poor), in which occurrences of plenty were observed.

The knitting and dyeing conditions were as follows. <Knitting conditions>-Warping draft: 2 times-Knitting machine: "28 gauge tricot" manufactured by KARL MAYER-Organization: Half (yarning front polyester, back polyurethane) ・ Number of on-board courses: 85 courses

<Dyeing conditions> Refining relaxation: 80 ° C. × 1 minute (continuous relaxer) ・ Preset: 180 ° C. × 40 seconds (pin tenter) ・ Dyeing Resolin Blue FBL (manufactured by Bayer) 2.5% owf Disper TL (Meisei Chemical Co., Ltd.) 1 g / l Bath ratio: 1:30 Temperature condition: The temperature was raised from 40 ° C. to 130 ° C. over 40 minutes, and maintained at 130 ° C. for another 30 minutes.

<Reduction washing> Hydrosulfite 2 g / dl Soda ash 2 g / dl Sanimol RC-100 (Nichika Chemical) 1 g / dl Conditions: 80 ° C. × 10 minutes <Finishing set> 170 ° C. × 45 seconds Finish density: 108 Course / in

REFERENCE EXAMPLE 1 part of a polyester polyol composed of 3-methyl-1,5-pentanediol and azelaic acid (purity: 99%) having a number average molecular weight of 2000, 4,4
'3.4 parts of diphenylmethane diisocyanate, 1,
4-butanediol was continuously supplied at a ratio of 2.3 parts to a twin screw extruder of 30φ, L / D = 36 by a metering pump, and continuous melt polymerization of polyurethane was performed at 240 to 260 ° C. Next, this was directly supplied to a spinning machine equipped with a single screw extruder, and a spinning temperature of 205 to 235 ° C, a cooling air dew point of 10 ° C,
Spinning is performed at a spinning speed of 500 m / min.
It was wound around a hollow cylindrical bobbin having a length of 5.3 mm, a length of 57.5 mm, and a thickness of 6.0 mm) to obtain a wound polyurethane elastic fiber of 40 denier / 1 filament (water content: 4000 ppm).

Example 1 A paper tube was made of aluminum foil (thickness 0.0
25 mm, the moisture permeability 0.3g / m ² / 24hr) at using a substrate made by coating winding yarn of Example (fiber moisture content 400
0 ppm, cheese diameter 30 mm, cheese width 40 mm)
After dehydration at 40 ° C. for 5 hours with a reduced pressure drier at a pressure of 1 torr to make the water content of the fiber 500 ppm, heat treatment was performed for 24 hours in a nitrogen gas at a dew point of −5 ° C. and a temperature of 90 ° C. Heat aging treatment was carried out by allowing to stand under relative humidity for 7 days. The obtained wound body had excellent hot water resistance and high homogeneity in the innermost layer and the outermost layer. Even when knitted and subjected to high-temperature dyeing, density unevenness and warping did not occur. Table 1 shows the results.

Example 2 A paper tube was made of aluminum foil (thickness 0.0
25 mm, the moisture permeability 0.3g / m ² / 24hr) at using a substrate made by coating winding yarn of Example (fiber moisture content 400
0 ppm, cheese diameter 30 mm, cheese width 40 mm)
Heat treatment was performed in a nitrogen gas at a dew point of + 15 ° C. and a temperature of 90 ° C. for 24 hours, followed by a heat aging treatment by leaving the mixture at a temperature of 25 ° C. and a relative humidity of 50% for 7 days. Table 1 shows the results.

[0037] [Comparative Example 1] paper tube moisture cellophane (thickness 0.040 mm, moisture permeability 50g / m ² / 24hr) at substrate made by coating using Reference Example winding yarn of (fiber moisture content 4
000 ppm, cheese diameter 30 mm, cheese width 40 mm)
Was dehydrated in a vacuum dryer at 40 ° C. for 5 hours at a pressure of 1 torr to make the water content of the fiber 500 ppm, and then the dew point was −5.
A heat treatment was performed for 24 hours in a nitrogen gas at 90 ° C. and a temperature of 90 ° C., and a heat ripening treatment was performed by leaving the substrate at a temperature of 25 ° C. and a relative humidity of 50% for 7 days. Table 1 shows the results.

[0038] [Comparative Example 2] The paper tube vinylidene chloride film (thickness 0.040 mm, moisture permeability 2.5 g ^/ m 2/24
hr) A wound body using a core body coated with the core material (fiber moisture content 4000 ppm, cheese diameter 30 mm, cheese width 40 m)
m) at 40 ° C. for 5 hours in a vacuum drier at a pressure of 1 torr to make the water content of the fiber 500 ppm, and then the dew point
Heat treatment was performed in a nitrogen gas at 5 ° C. and 90 ° C. for 24 hours, and then left at 25 ° C. and 50% relative humidity for 7 days for heat aging. Table 1 shows the results.

[0039] [Comparative Example 3] paper tube moisture cellophane (thickness 0.040 mm, moisture permeability ^50g / m 2 / 24hr) winding yarn body winding yarn body using substrate made by coating with (fiber moisture content 40
(00 ppm, cheese diameter 30 mm, cheese width 40 mm)
Was dehydrated in a vacuum dryer at a pressure of 1 torr at 40 ° C. for 5 hours to make the water content of the fiber 500 ppm, and then the dew point was +15.
A heat treatment was performed for 24 hours in a nitrogen gas at 90 ° C. and a temperature of 90 ° C., and a heat ripening treatment was performed by leaving the substrate at a temperature of 25 ° C. and a relative humidity of 50% for 7 days. Table 1 shows the results.

[0040] [Comparative Example 4] The paper tube vinylidene chloride film (thickness 0.040 mm, moisture permeability 2.5g / m ^2/24
hr) A wound body using a core body coated with the core material (fiber moisture content 4000 ppm, cheese diameter 30 mm, cheese width 40 m)
m) in nitrogen gas at a dew point of + 15 ° C and a temperature of 90 ° C for 24 hours.
After heat treatment for a period of time, the mixture was left at a temperature of 25 ° C. and a relative humidity of 50% for 7 days to carry out heat aging treatment. Table 1 shows the results.

[0041]

[Table 1]

[0042]

According to the present invention, a wound body having high heat resistance and water resistance in the innermost layer and excellent homogeneity in the same cheese can be obtained. When high-temperature dyeing or high-temperature high-pressure dyeing is performed, a high-quality fibrous structure can be obtained without occurrence of density unevenness, warping, or the like.

 ────────────────────────────────────────────────── ─── Continued on the front page F term (reference) 3B154 AA06 BA07 BA60 BB12 BC18 BE01 BF01 BF03 BF13 BF15 DA02 DA13 DA16 4H057 AA02 BA81 DA01 DA22 DA31 HA01 JA10 JB02

Claims (5)

[Claims] 1. A method for heating and aging polyurethane elastic fibers, comprising subjecting a wound body obtained by winding a polyurethane elastic fiber obtained by a melt spinning method to a core having at least a surface made of aluminum and subjecting it to a heat aging treatment. 2. A wound body obtained by winding a polyurethane elastic fiber obtained by a melt spinning method on a core body of which at least the surface is made of aluminum has a dew point of -20 ° C.
A method for heating and aging polyurethane elastic fibers, wherein the heating and aging treatment is performed in a gas at + 25 ° C and a temperature of 50 to 100 ° C. 3. A polyurethane elastic fiber or a polyurethane elastic fiber obtained by subjecting a wound body obtained by winding a polyurethane elastic fiber obtained by a melt spinning method to a core body having at least a surface made of aluminum and subjecting it to a heat aging treatment. A method of performing high-temperature dyeing on a fibrous structure containing elastic fibers. 4. A polyurethane elastic material which is wound around a core body after spinning by a melt spinning method, wherein the innermost layer of the wound body has a residual distortion after heat-resistant water treatment of 67% or less. Fiber wound body. 5. The fiber according to claim 4, wherein the difference in the relative viscosity of the fibers between the innermost layer and the outermost layer of the wound body is 0.01 to -0.03.
3. A wound polyurethane elastic fiber according to claim 1.