JPS609909A - Nylon 66 fiber having excellent level dyeing property and its manufacture - Google Patents

Abstract

PURPOSE:To manufacture the titled fiber having particular fine structure and excellent level-dyeing property, by melt-spinning nylon 66, steaming the fiber with a specific amount of steam using a steam-conditioning column having a specific length, winding at a low speed, and drawing the obtained fiber. CONSTITUTION:Nylon 66 polymer is melted and extruded from the spinneret 1, and cooled with chilled air between the heat-insulation cylinder 2 and the inlet of the steam-conditioning column 4. Steam is applied to the fiber at a rate of <=5g/min with the steam-conditioning column 4 having a length of <=30cm, and wound with the winder 9 at a winding rate of <=1,200m/min. The objective fiber manufactured by this process has a diffraction intensity ratio (R) of the reflection at 2theta=11 deg. to that of (010)+(110) plane of >=0.8, the apparent crystal size (ACS) obtained from the reflection of the (100) plane of >=85%, and a crystal perfection index (CPI) of >=55% measured by X-ray diffraction intensity measurement.

Description

DETAILED DESCRIPTION OF THE INVENTION Technical Field The present invention relates to nylon 66 fibers with excellent level dyeing properties. More specifically, the present invention relates to nylon 66 fibers that have a special fine structure, have excellent level dyeing properties, and have good structural stability at high temperatures.

Conventional technology Nylon 66m fiber is among the polyamide fibers and has excellent strength, durability, and elasticity, and is easy to dye in vivid colors, so it is used for various clothing applications, especially as a dyestuff. By dyeing with metal-containing dyes, vivid dyed products with excellent fastness can be obtained. However, dyed products obtained using these dyes with excellent fastness have the disadvantage that dyeing is difficult and staining spots are more likely to occur compared to nylon 6 fibers. For this reason, efforts have been made to strengthen manufacturing controls, such as extremely strict control of conditions in the spinning, stretching, and processing processes, and prior dyeing and sorting of raw yarn before or after processing, but this is still insufficient. However, such enhanced control is extremely disadvantageous from the viewpoint of manufacturing costs.As a method to improve these drawbacks of nylon 66 fiber, a method is known in which nylon 6 is mixed with nylon 66 and copolymerized. Although this method improves the level dyeing properties of the resulting fibers, it has the disadvantage that the thermal properties and mechanical properties of the nylon 66 fibers deteriorate due to the copolymerization of nylon 66. On the other hand, 3.000 m of nylon 66
It is known that intermediately oriented yarns obtained by spinning at a speed of about 5,000 m/min to 5,000 m/min are drawn and false-twisted, and dye spots are relatively reduced. The residual elongation of these fibers is high, and the drawing ratio has to be increased during false twisting, making it difficult to control the difference between processing weights, which may also cause problems such as a decrease in the dyeing fastness of the processed yarn and a decrease in the texture of the processed yarn. The problem arises.

In general, the dyeability of polyamide fibers is determined by the amine end groups and fine structure when dyeing with the aforementioned acid dyes and metal-containing dyes, and by the fine structure when dyeing with disperse dyes. In particular, the level dyeing property is greatly influenced by the fine structure and its variations. Furthermore knife 266
Compared to nylon 6 fibers, m-fibers have a larger hydrogen bonding capacity, and therefore are more likely to undergo microstructural changes due to moisture absorption, etc., which tends to widen the variation and have poor level dyeing properties.

Summary of the Invention The present inventors analyzed how the microstructure of nylon 66 fibers changes over time due to moisture absorption, heat history, etc., and found that the changes over time in the microstructure are similar to those of crystals. We found that the rate-determining step is the change in temperature over time, and investigated this.

As a result, it was confirmed that the fine structure of the fibers immediately after production has extremely grown crystal parts, which greatly suppresses changes in the crystal parts over time due to WK turbidity, heat history, etc. after production. The present invention has been achieved based on the discovery that the level dyeing property is significantly improved by using the above-mentioned method.

That is, in the present invention, in X-ray diffraction intensity measurement, (1)
The ratio (R) of the diffraction intensity of the reflection of 2θ=110 to the diffraction intensity of the reflection of the (olo) + (110)) plane is 08 or more, and the apparent The size of microcrystals (A OS) is 60f or more, (1
The present invention relates to a nylon 66 fiber with excellent level dyeing properties, which is characterized by having a crystal orientation (C○) of the 00) plane of 85% or more and a crystal perfection (OP) of 55% υ or more.

In the present invention, nylon 66 refers to Bo1J hexamethylene adipamide polymerized from hexamethylene diamine and adipic acid, and a small amount of commonly used additives,
For example, it may contain a quenching agent, an antistatic agent, a stabilizer, a terminal regulator, etc., and a small amount of a copolymer component within a range that does not deteriorate the physical properties of nylon 66.

A particularly important feature of the fibers of the invention is that they have a novel crystal structure. This crystal structure will be explained in detail below.

FIG. 1 is a diagram of a diffraction intensity distribution curve in the equatorial direction obtained by measuring the X-ray diffraction intensity of nylon 66 fiber.

From the low angle side of the diffraction angle 2θ, the diffraction intensity peak of the reflection at 2θ = 11°, the diffraction intensity peak of the reflection of the (100) plane, (
The diffraction intensity peak of reflection from the (olo)+(11o)) plane is shown. The solid line curve (1) in FIG. 1 illustrates the diffraction intensity distribution curve of the fiber of the present invention, and the dashed line curve (2) illustrates the diffraction intensity distribution curve of the conventional nylon 66 fiber. This X
Details of the linear diffraction intensity measurement will be described later. As is clear from Figure 1, in the conventional nylon 66 fiber (curve (2)), the reflection seen near the diffraction angle 2θ = 11° is small, and
2 for the diffraction intensity of reflection on the 010)+(110)) plane
The ratio (R) of the diffraction intensity of reflection at θ=11° will never exceed 0.8. On the other hand, in the fiber of the present invention (curve (1)), the reflection seen near 2θ = 11° is extremely large, and the reflection at 2θ = 110 with respect to the diffraction intensity of the reflection from the ((010) + (110) plane is extremely large. Ratio of diffraction intensity of reflection (R)
is 0.8 or more, which is much larger than conventional fibers.

In order for conventional nylon 66 fibers to have stable and large crystals in their microstructure, it is necessary to use high viscosity polymers in the spinning process, increase the draw ratio in the drawing process, and apply heat setting. However, the elongation of the resulting fibers becomes low and the dyed product becomes light dyed, resulting in a decrease in dyeing quality. However, because the fiber of the present invention has an R of 0.8 or more, its AO8, OF, and 00 values are higher than conventional fibers, and although it is extremely stable and has large crystals, its elongation is reduced. This eliminates problems such as fuzz generation and thread breakage during post-processing processes such as net making, weaving, and false twisting, as well as problems such as deterioration of dyeing quality due to lighter dyeing of dyed products. does not occur,
The level dyeing property is also excellent.

Therefore, it is extremely surprising that we were able to develop a stable crystalline structure that does not undergo changes over time in the fine structure of the fibers without causing the above-mentioned troubles. The fiber of the invention has extremely excellent level dyeing properties.

Various parameters expressing the microstructure of the crystalline part of the fiber (
The size of the microcrystal on the (100”) plane is AO8), (100
) plane crystal orientation (Co) and crystal perfection (OP) are related to the mechanical properties (strength and elongation, initial modulus) and thermal properties (dimensional stability, stability of microstructure against heat) of the fiber. do. In the fiber of the present invention, AO8 and OO are preferred in terms of providing satisfactory strength and elongation, modulus, and dimensional stability as well as thermal microstructural stability for use in clothing.
are preferably 30A or more and 85% or more, respectively. More preferable values of these parameters are 35λ or more and 88% or more, respectively. AO8 is 30
If it is smaller than Cheap. On the other hand, when 00 is smaller than 85%, the initial elastic modulus decreases easily during heating.

Furthermore, in order to improve the dimensional stability of the fibers and to reduce the decrease in the initial elastic modulus when subjected to heat, it is preferable that the OP ratio is 55% or more. When the OP is 55% or less, the amount of irreversible decrease in elastic modulus associated with temperature rise tends to be large.

Here, parameters such as AO8.00 and OP are measured using the X-ray diffraction method described later.

In the fiber of the present invention, the fine structure not only has a stable crystalline structure that does not change over time, but also has stable mechanical loss, which greatly increases the level dyeing property.

In other words, the peak value (tanδmaw) of tanδ of α4 absorption in the mechanical loss tangent (tanδ)-temperature (T) curve and its temperature position (TIIILX) are 0.08≦tanδwax≦0.12 110C≦Tmax≦120C It is preferable.

Since the fiber of the present invention has an extremely stable crystal structure,
Although there is little change in the microstructure over time, t&nδmax and T
When max satisfies the above-mentioned range, changes in the fine structure over time are further dramatically suppressed and level dyeing properties are improved.

The correlation between the dyeability of nylon 66 fibers and the tan δ-1 curve is that the magnitude of the absorption (αα absorption) that appears due to the micro-brown interaction of the primary mirror and the dyeability (equilibrium dyeing amount) are almost positive. It is known that there is a correlation. However, there is not necessarily a difference between the size of the equilibrium dyeing amount and the quality of dye suppression.
There is no one-to-one correlation. It was generally thought that the higher the TlfIaX content, the smaller the degree of change over time in the fine structure, which is one of the factors for the decline in level staining. Therefore, in order to reduce microstructural changes and improve level dyeing, it has been necessary to increase Trnax. As a method for increasing TIIILX, increasing the stretching ratio is generally adopted. If a high draw ratio is adopted, T max will certainly increase, and as a result, changes in the microstructure over time will be reduced, but on the other hand, tan-a-wax will decrease, dyeability (equilibrium dyeing amount) will decrease, and the draw ratio will increase. Further increase T m
On the contrary, when ast exceeds 120C, the level dyeing property decreases.

Therefore, Tmax is 11, OC≦T! II! It is preferable that LX≦120C.

Furthermore, if tan δwax is smaller than 0.08, the dyeability (equilibrium dyeing amount) decreases, resulting in light dyeing and decreasing dyeing quality. On the other hand, if it is larger than 0.12, the dyeability (equilibrium dyeing j1
), but the dimensional stability and thermal stability of the microstructure decrease. Therefore, tan δmax preferably satisfies the following: 0.08≦tan δm&X≦0.12.

The fibers of the present invention as described above are obtained by melt-spinning nylon 66 polymer and winding it as an undrawn yarn, using a steam conditioner, a column length of 30 scratches or less, a steam amount of 51/min or less, and a speed of 1200 m/min. The manufacturing method of the present invention will be described in detail below.

Generally, an undrawn yarn of nylon 66@ fiber is moistened by the humidity of the winding atmosphere, so the elongation rate (Δt) of the undrawn yarn immediately after winding is high. Because this Δt is large, the fine structure of the undrawn yarn immediately after winding is! Changes occur over time with g-moisture, and the variation becomes large. therefore,
The lower the Δt of the undrawn yarn of nylon 66m fiber, the less the undrawn yarn changes over time, and the smaller the variation, the less the variation in the microstructure of the fiber obtained by drawing the undrawn yarn, and the higher the level dyeing. It was also considered to have excellent sex. Therefore, the Δt of undrawn yarn of nylon 66 fiber is usually set to 2% or less. Conventionally, when winding undrawn yarn of nylon 66@fiber, the amount of steam is set to 5, off for 1 minute or more so that Δt is 2% or less, and excess water vapor is applied with a steam conditioning column. Alternatively, Δt has been suppressed by increasing the winding speed to increase the birefringence Δn of the undrawn yarn and perfecting the fine structure of the undrawn yarn. However, the manufacturing method of the present invention is a manufacturing method that is completely different from the above-mentioned conventional technology, and Δt of the undrawn yarn does not need to be 2% or less. Note that steam here refers to saturated water vapor at normal pressure and high temperature.

A feature of the production method of the present invention is that when melt-spinning nylon 66 polymer and winding it as an undrawn yarn, the amount of water added is extremely small compared to the conventional method. the length of 30a
m or less, the steam amount is 51/min or less, and 1200 m/min or less.
The purpose is to wind the film at a winding speed of less than 1 minute. By stretching such undrawn yarn according to a conventional method, the nylon 66 fiber of the present invention having excellent level dyeing properties can be obtained.

The Δt of the undrawn yarn obtained by the production method of the present invention is larger than that of the undrawn yarn of conventional fibers, and it is extremely easy to swell.
Despite large changes over time, the fine structure of the fibers obtained by drawing such undrawn yarns exhibits a stable crystalline structure that is difficult to change over time, resulting in nylon 6 with extremely excellent level dyeing properties.
The fact that 6@fibers can be obtained is an extremely surprising effect that could not be predicted from the conventional techniques.

When making the Δt of the undrawn yarn larger than the Δt of the undrawn yarn of conventional fibers, the Δt is the same as the Δt immediately after winding the undrawn yarn.
In relation to n, it is preferable to satisfy the condition Δt≧3X122Δn−1. In FIG. 2, the range of the above formula is shown with diagonal lines. In the figure, the vertical axis represents the elongation rate of the undrawn yarn immediately after winding, and the horizontal axis represents the birefringence index of the undrawn yarn immediately after winding.

It is preferable to provide a slot in the filament introduction part of the steam funding column to reduce water vapor leaking upward from the introduction part.

Further, it is also possible to remove the steam conditioning column and the wrapping column within the range of not causing defects in the shape of the winding pad and stage of the undrawn yarn.

FIG. 3 shows an example of an undrawn yarn winding and spinning facility for obtaining invention #DJ fiber. 4 in Fig. 3 is the steam conditioning column.

A plurality of multifilaments F may be introduced into the steam conditioning column at the same time.

The fibers of the present invention can be used as processed yarns or as filaments as they are for knitting, fabrics, and other clothing applications.In addition to the level dyeing properties of the fibers themselves, they are also resistant to fluctuations in conditions during the processing process, and are therefore extremely stable. A product with excellent level dyeing properties and fewer dye spots can be obtained.

The methods for measuring the structural properties and other properties of fibers used in the present invention will be described below.

(Apparent microcrystal size AC+8)) X in the equator direction
By measuring the line diffraction intensity using the symmetric reflection method,
You can install the program O8.

XNa@ fractal intensity was measured using Rigaku Denki Co., Ltd.'s RU-200Pi and goniometer (SG-91), a scintillation counter for the meter and tube, and a pulse height analyzer for the counting section. OukαsI(λ=1.
5418A).

Place the fiber sample on an At sample holder so that the fiber axis is perpendicular to the folding surface. At this time, the thickness of the sample should be about 0.5 snow.

Operating the xIiI generator at 50 KVs 80 mA, scanning speed 2θ, 1°/ynis, chart speed 10 1/111 s time constant 1
seconds, divergence pickpocket, ) 1/2°, receiving pickpocket, ) 0.3 snowball, scan, tarring pickpocket, ) 1
/2° and record the diffraction intensity at a diffraction angle 2θ of 7° to 35°. The full scale of the recorder is set so that the resulting diffraction intensity curve falls within the scale, and is set so that at least the maximum intensity value does not exceed 50% of the full scale.

The fibers of the present invention are characterized by having two main reflections generally in the range of equatorial diffraction angles 2θ = 20.0° to 2465° (low angle side is (100) plane, high angle side is (010) + (11
0) surface). The method used to calculate AO8 is, for example, the formula of -11, "X@Diffraction of Polymers" by Alexander, Kagaku Dojin Publishing, Chapter 7, 5aherrer.

The diffraction intensity curves between 2θ=70 and 35° are connected by a wire and used as a base line. Draw a perpendicular line from the peak of the diffraction peak to the baseline, and mark the midpoint between the peak and the baseline. g]< between the diffraction intensity curves with a horizontal line passing through the midpoint.

This line intersects two shoulders of the peak of the curve if the two principal reflections are well separated, but only one shoulder if the separation is poor. Measure the width of this peak. If it intersects only one shoulder, measure the distance from the intersection to the midpoint and double it. If it crosses two shoulders, measure the distance between them. These values are converted into radians and used as the line width. Furthermore, this line width is corrected by the following method.

β=Q-B is the measured line width, b is the P4-donning constant &81
This is the line width (half width) expressed in radians of the peak of (111) plane reflection of a single crystal. The apparent size of microcrystals is given by the following formula. Here, X is 1, and λ is the wavelength of XH (
1,5418A), β is the corrected line width, and θ is the positive angle, which is 1/2 of 20.

(Crystal orientation degree (00)) The crystal orientation degree of the fibers was measured using a Rigaku Corporation XLS generator (RU-200P L), a fiber +1i [Nil constant device (PS-5), a goniometer (SG-9), A scintillation counter is used for the counter, a pulse height analyzer is used for the counting section, and 2. Oukα is made monochromatic by a Kel filter.
(λ=1.54181).

The fibers of the invention are generally characterized by having two major reflections on the equator. 00@ constant uses a reflection with a low angle of 2θ. 20 of the reflections used are determined from the diffraction intensity white line in the equatorial direction.

The xfi1 generator operates at 30 KV s 80 mA.

Attach the sample to the fiber sample measuring device so that the single threads are parallel to each other. The thickness of the sample is 0.5 snow ■
It is appropriate to make it so that The goniometer is set to the 2θ value determined from the equatorial diffraction intensity curve. Using the symmetrical transmission method, the azimuth direction is set from -300 to +
300 scans and record the diffraction intensity in the azimuthal direction. Furthermore, the diffraction intensity in the azimuth directions of -180° and +180° is recorded. At this time, the scanning speed was 4°/ln, and the chart speed was 1011/wuR.

Time converter: 21 fsec, collimator: 2mmφ, receiving pick, vertical width: 1.91111% width: 3.5 I
O which is II To subtract 00 from the obtained diffraction intensity curve in the azimuthal direction, take the average value of the diffraction intensities obtained at ±180C, draw a horizontal line, and use it as a base line. Draw a perpendicular line from the top of the bead to the base line and find the midpoint of its height. Draw a horizontal line through the midpoint,
The distance between the intersection of this horizontal line and the I1gI flexural intensity curve is measured, and the value obtained by converting this value into an angle (0) is defined as the orientation angle H.

The degree of crystal orientation is expressed by the following formula %formula% given by.

[Crystal perfection (OP)]

For the measurement of crystal perfection (OP), an X-ray diffraction intensity curve obtained from the AO8 measurement method is used.

To measure crystal perfection (OF), use Dismore and 5
Tatton's method is used.

The OP is given by the following equation.

Here, A is 0.189, and the closer the OP value is to 100, the higher the degree of crystal perfection.

(1010)+(110)) Ratio of the diffraction intensity of reflection at 2θ=11° to the diffraction intensity of reflection at the (110)) plane] A mentioned above
In the X-ray diffraction intensity measurement curve measured when measuring O8, a straight line connects the diffraction intensity curves at diffraction angles 2θ=7° and 35° and is used as a baseline.

((010)+(110)) plane reflection and 2θ=11
For the diffraction intensity of the reflection at 100°, a perpendicular line is drawn from the apex of the diffraction peak to the base line, and the diffraction intensity between the peak and the base line is obtained. And R is given by the following formula.

[Mechanical loss tangent (ta・nδ)]

To measure the mechanical loss tangent (tan δ), a VIBRON DD'V-TIQ model manufactured by Toyo Baldwin Co., Ltd. is used. The tan δ - temperature (T) characteristics are measured in dry air at a measurement frequency of 1oc/=. From the tan δ-temperature curve, t
The andδ peak height tanδmAX and the tanδ peak temperature Tmax (C) are obtained.

(Birefringence (Δn)) To measure the birefringence, a transmission interference microscope manufactured by Karl Zeiss Jena, East Germany is used. At a wavelength of 549μ and a temperature of 25C, the birefringence △n is given by the refractive index ``11'' for light vibrating parallel to the fiber axis and the refractive index nL for light vibrating perpendicular to the fiber axis. Δn = n11- nl.

It is expressed as

Note that the center of the fiber is defined as the center of gravity when the fiber cross section is considered to be one plane for both circular cross-section and irregular cross-section fibers.

[Elongation rate (Δt)] One end of a fiber having a sample length t1 is gripped by a sample gripping claw, a load of 151 F/denier is tied to the other end, and the fiber is hung vertically from the sample gripping claw. After 30 minutes, the sample length t2 is measured and Δt is calculated according to the following formula.

Note that the measurement atmosphere was 2DC, na 70%. Also, t
,=1m.

(Relative viscosity (VR)) Dissolve 8.4% nylon 66 in a 90% formic acid solution and measure at 25C by a conventional method.

[Incidence rate of staining spots]

The processed yarn obtained by false twisting the sample was made into a tubular knitted fabric, and Diac
id A11zr4n Light Blue 4 G
L 0.5% owf, acetic acid and ammonium acetate were added to adjust the pH to 5.0, the temperature was raised from room temperature to 980 in 60 minutes, kept at 98C for another 10 minutes, and then lowered to obtain a dyed knitted fabric. , the presence or absence of dye spots is determined visually. The incidence of staining spots is shown in the margin below.

[Level dyeing]

From the obtained sample, a half-trift was formed using 52 GG, and after scouring and presetting at 160r x 30mm, it was dyed using a Weins dyeing machine, Suminol Mill Br1ll, Blue.
G (Sumitomo Chemical product) 0.5% ovf, vinegar ammonium 6% owf.

Dyeing was carried out at a bath ratio of 1150, a boiling time of 60 minutes, and a heating rate of 30'C to a boiling temperature of 2C/#.

Visually judge the dyed fabric according to the following criteria, and check the level of dyeing (collection/discharge).
Assessed the level. Judgment was made on a five-point scale, with 5th grade being where no collection or discharge was observed, 3rd grade if some collection or discharge was observed, and 1st grade if significant collection or discharge was observed. Moreover, those at each intermediate stage were classified as 4th grade and 2nd grade.

[Strong elongation]

Manufactured by Toyo Baldwin, TKNSLLON UTM-
It was measured by a conventional method using a 17-20 type tensile tester.

Note that the measurement atmosphere was 20rbRu60%.

Example The present invention will be further explained below using Examples.

Example 1 Using the spinning equipment shown in Fig. 3, a relative viscosity (VR) of 4
0.0 nylon 66 at a spinning temperature of 290C with a pore diameter of 0.20
tu, melt-spun from spinneret 1 with 24 holes, heat-insulating tube 2
Cooling is performed with 2DC cooling air between the inlet of the steam conditioning column 4 and the inner diameter is 180! II. Steam was applied in a steam conditioning column 4 with a length of 10 cm to 200 onL, and a finishing agent of 15% concentration was applied in a low/I/8 with a roughness of 3 seconds and an outer diameter of 130 mm rotating at 5-speed. The undrawn yarn was wound at a winding speed of , 800 m/min. After that, according to the usual method, the drawing ratio was 3.5.
A drawn yarn of 70 denier/24 filaments was obtained. Note that steam (saturated water vapor of about 102C) is introduced into the steam conditioning column 4 through a steam introduction pipe 5, and excess moisture is continuously removed by a drain vibro. In this example, the amount of steam was adjusted to 517 minutes using the steam introduction pipe 5. Δn of the obtained undrawn yarn.

Table 1 shows ΔL, the microstructural characteristics, and the dyeing characteristics of the obtained drawn yarn.

In Table 1, Nh1 to Nh3 are the fibers of the present invention, especially Nh
N1 and N2 are examples of fibers within the preferred range of the present invention, and exhibit excellent dyeing properties and level dyeing properties. On the other hand,
NQ4 to NQ6 are examples of fibers that have unstable crystal structures and are outside the scope of the present invention, and are inferior in dyeing properties and level dyeing properties compared to NQ1 to NQ6.

The following is Yomi Table 1 Example 2 The fibers -1 to 6 obtained in Example 1 are 20C1RH=60
% temperature and humidity for 5 units (indoors) for 60 days, the crystal structure characteristics, streak occurrence rate, and level staining were measured. The results are shown in Table 2.

In Table 2, the fibers-1 to N116 of the invention examples still exhibit excellent dyeing properties and level dyeing properties. However, in the fibers of Comparative Examples Nos. 4 to 6, the OP process increased, and the crystals in the microstructure gradually grew. The dyeability is also far inferior to the value of Example 1 60 days ago.

The following margin Example 3 Under the same spinning conditions as floor 2 of Example 1, only the amount of steam was 0.
~50? /min to obtain an undrawn yarn, which was drawn in a conventional manner to obtain a drawn yarn of 7o denier/24 filaments. Table 3 shows Δn1Δt1 of the obtained undrawn yarn, and the microstructural characteristics and dyeing characteristics of the obtained drawn yarn.

In Table 3, grades Nn7 to 9 are examples of the fibers of the present invention, which have extremely excellent dyeability and level dyeability.

On the other hand, in the case of positive 10 to 11, the amount of steam increases and the fiber of the present invention falls outside the microstructure range of the present invention, and the fiber of the present invention cannot be obtained.
The dyeing properties and level dyeing properties are inferior to that of .

The following margin is Table 3 Implementation [4] Under the same spinning conditions as in floor 2 of Example 1, only the winding speed of the undrawn yarn was changed from 600 m/min to 4,000 m/min to obtain an undrawn yarn, When drawing each of these undrawn yarns, the drawing ratio was adjusted so that the elongation of the drawn yarn was 30 to 35%, which can withstand practical properties, and the drawn yarn was drawn according to a conventional method to obtain a drawn yarn of 70 denier/24 filaments. Obtained. Table 4 shows the drawing conditions for ΔY and Δ of the obtained undrawn yarn, as well as the microstructural characteristics and dyeing characteristics of the obtained drawn yarn.

In Table 4, shade 12 to grade 13 are the fibers of the present invention, which have extremely excellent dyeing properties and level dyeing properties.

On the other hand, in the case of Nn14 to 15, the winding speed of the undrawn yarn increases and the fiber of the present invention falls outside the range of the fine structure of the fiber of the present invention, and the fiber of the present invention cannot be obtained. The dyeing properties and level dyeing properties are poor.

Margin below

[Brief explanation of drawings]

Figure 1 shows the diffraction intensity distribution curves in the equatorial direction obtained by X-ray diffraction analysis of the fiber of the present invention and the conventional fiber. ◇Figure 2 shows the Δn and Δt of the undrawn yarn to obtain the fiber of the present invention range(
The shaded area) is shown. FIG. 3 is a drawing of a spinning facility showing an embodiment of the spinning process of the present invention. A brief explanation of each drawing is provided below. Figure 1 (1)... Xi1 diffraction intensity distribution curve of the fiber of the present invention (
2)...Second X111 diffraction intensity distribution curve of conventional fiber
m Shaded area: Δn of undrawn yarn to obtain the fiber of the present invention
and Δt range 3rd v! J 1... Spinneret 2... Heat retention tube 3... Spun yarn 4... Steam conditioner, Eng column 5... Steam introduction pipe 6... Drain pipe 7... Yarn running guide 8... Finishing agent 4 - 9... Winding machine Patent applicant Asahi Kasei Kogyo Co., Ltd. Patent agent Akira Aoki Patent attorney Kazuyuki Nishidate Patent attorney Tsuyoshi Yoshida Patent attorney Akiyuki Yamaguchi Figure 1 Diffraction angle 2θ (°) Figure 2 Birefringence (Δn) Figure 3 Procedural amendment (voluntary) 1982! Kazuo Wakasugi, Commissioner of the Tsukinohi Patent Office1, Indication of the case, Patent Application No. 112613 of 1982, Name of the invention, Nylon 66 fiber with excellent level dyeing properties and its manufacturing method, 3, Person making the amendment, and Relationship Patent applicant name (003) Asahi Kasei Kogyo Co., Ltd. 4, agent address 5-8-10 Toranomon-chome, Minato-ku, Tokyo 105
Column 6 of "Detailed Description of the Invention" of the specification to be amended, content of amendment 0) We will correct the following errors in each of the following in the specification. (b) Page 26 of the specification, column R in Table 1, ro, 145
Correct J to Ir1.45J, rO, 105J to rl, 05J. (-Now, in Table 1 on page 26 of the specification, ``Streae incidence rate (H)'' has been corrected to ``R streak incidence rate (CH).'') Page 28 of the specification, 2 Column R in the table, rO, 148J
RL that says 48J, RL that says "0.103"
, corrected to 03J. 2) "Streae incidence rate (H)" in Table 2 on page 28 of the specification
Correct the statement to "striae incidence (%)". (to) Page 30 of the specification, column R in Table 3, ro, 148
J toraru to rl, 48J to rO, 120J to r
Correct "l, 20J, ro, ro8" to rl, 08J. (g) In Table 3 on page 30 of the specification, “Streae incidence (ch)
" is corrected to "Striae incidence (chi)". (a) Page 32 of the specification, column R in Table 4, ro, 1xo
” to rl, 10J to ro, 096J toal to r
o, 96J, ro, oso" is corrected to rO, 60J, and rO, 043J is corrected to r O, 43J. (Male Specification page 32, Table 4, ``Striae incidence (%)
Correct "Toruru to 1 staining spot incidence (chi)". (Closed) The formula at the top of page 20 of the specification will be amended to the following formula. "

Claims (1)

[Claims] 1. In X-ray diffraction intensity measurement, ((010)+(11
0)) The ratio (R) of the diffraction intensity of reflection at 2θ = 11° to the diffraction intensity of reflection of the surface is 0.8 or more, and (100)
Apparent microcrystal size A determined from surface reflection
(78) is 30x or more, crystal orientation degree of (100) plane (0
Nylon 66 fiber with excellent level dyeing properties, characterized by having 0) of 85% or more and crystal perfection (OP) of 55% or more. 2. In dynamic viscoelasticity measurement, mechanical loss tangent (tan
δ) The peak value (tanδwax) of tanδ of αa absorption in the temperature (T) curve and its temperature position (Tmax) are as follows: 0.08≦tamJmax≦0.12 110C≦Tm1LX≦1.20C Nylon 66 fiber according to item 1. 3. Steam conditioning is used when melt-spinning nylon 66 polymer and winding it as undrawn yarn. The length of the cooking column is 30 mm or less, and the steam amount is 5 fI.
A method for producing nylon 66 fiber with excellent level dyeing properties, which comprises winding the yarn at a winding speed of 1200 m/min or less, and drawing the resulting undrawn yarn according to a conventional method.