JPH0860541A - Yellowing-resistant polyamide-based fiber structure and its production - Google Patents

Abstract

PURPOSE: To obtain a yellowing-resistant fiber structure excellent in preventing effects on yellowing rich in durability to an extent so as not to visually observe the yellowing of the fibers without adversely affecting the hue of a dyed product by treating a polyamide-based fiber structure with a specific acid anhydride. CONSTITUTION: This yellowing-resistant polyamide-based fiber structure is obtained by treating a polyamide-based fiber structure such as nylon 6 or nylon 66 with a vapor phase and/or a liquid phase of an acid anhydride (the acid anhydride which is 100% liquid phase), preferably acetic anhydride, e.g. in the vapor phase or according to a dipping method. Thereby, the yellowing-resistant polyamide fiber structure, causing yellowing which is ΔYI<1 visually unconfirmative yellowing index thereof with vanillin and excellent in durability is safely obtained at a low cost. As a result, the polyamide-based fiber structure, having the dyeability preferably within the range of -5<Δ L<5, excellent in properties of preventing the yellowing even after scouring and dyeing without causing the deterioration in dyeability and adversely affecting the hue by dyeing the fiber structure is obtained.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to prevention of yellowing of polyamide fibers, and relates to a polyamide fiber structure which is excellent in yellowing prevention and has good dyeability and does not yellow, and a simple and safe production method. .

[0002]

2. Description of the Related Art Heretofore, as a method for imparting a yellowing preventing effect to a polyamide fiber, a method has been proposed in which a terminal amino group is ionically bound.

However, the method of blocking the terminal amino group by an ionic bond has a problem that if it is carried out before dyeing, the yellowing preventing effect is lowered by the dyeing or the yellowing preventing effect is completely eliminated.

In addition, prevention of yellowing by ionic bonding is usually
Since it is carried out at the same time as or after dyeing, and it binds with the same mechanism as the dye, it may affect the dyeability, and there is a problem that the treatment with a concentration that does not affect the dye has a low ability to block amino groups.

Further, as a method for imparting a yellowing-preventing effect to a polyamide fiber, a method of treating a terminal amino group with a solution containing an acylating agent has been proposed in JP-A-4-272270.

However, this method has a problem that it is difficult to block amino groups to the extent that dyeing properties are not affected, and the coloring property is low.

[0007] Further, there is no defense against yellowing during the storage period, and it is very difficult to perform such a treatment in a greige since it is also a treatment in a bath.

Regarding the yellowing during the storage period, measures have been taken to shield it from the yellowing substances by packaging it with a high-density film, but if the package breaks, the yellowing will occur from the location and the subsequent steps The current situation is that there is a problem.

[0009]

DISCLOSURE OF THE INVENTION The present invention solves the above-mentioned drawbacks of the prior art, is excellent in yellowing-preventing property, and has good dyeability, and a yellowing resistant polyamide fiber structure, and a simple and safe production. To provide a method.

[0010]

In order to achieve the above object, the present invention has the following constitution.

That is, the yellowing-resistant polyamide fiber structure is characterized in that the yellowing of the polyamide fiber structure due to vanillin is ΔYI <1.

The method for producing a yellowing resistant polyamide fiber structure of the present invention has the following constitution.

That is, it is a method for producing a yellowing-resistant polyamide fiber structure, which comprises treating the polyamide fiber structure with a gas phase and / or a liquid phase of an acid anhydride.

[0014]

The yellowing resistant polyamide fiber structure of the present invention and the method for producing the same will be described in detail below.

In the present invention, the yellowing of the polyamide fiber structure due to vanillin is yellowing due to a yellow substance formed by binding a terminal amino group of the polyamide fiber and vanillin to form a conjugated system.

ΔYI is a difference in YI value, which is a degree of yellowing measured by an optical means, and is a polyamide colored yellow by a yellow substance formed by bonding of vanillin with a polyamide fiber having no binding with vanillin. The color difference of the system fibers is shown. The larger this value, the greater the degree of yellowing and incomplete blocking of amino groups, and the smaller this value, the lesser degree of yellowing and the closer the blocking of amino groups is to perfection.

In the yellowing resistant polyamide fiber structure of the present invention, ΔYI <1.

In the fibrous structure of the present invention, regardless of whether it is undyed or dyed, at least one of them may satisfy ΔYI <1.

When ΔYI ≧ 1, there is a problem that the degree of yellowing is increased and the hue of the cloth is affected.

ΔYI <1 is a degree of yellowing that cannot be visually confirmed, and is a degree of yellowing that does not affect the hue after dyeing even if it is dyed. Thus, the Δ of the fabric
By keeping YI <1, a high yellowing prevention property can be exhibited.

Next, in the yellowing resistant polyamide fiber structure of the present invention, the coloring property ΔL by dyeing is the lightness L value of the standard cloth measured by optical means and the polyamide fiber treated with an acid anhydride. The difference from the lightness L value of the structure is shown.

From the viewpoint of not deteriorating the color developability, the yellowing resistant polyamide fiber structure of the present invention is -5 <ΔL.
A range of <5 is preferable.

Next, a method for producing the yellowing resistant polyamide fiber structure of the present invention will be described. The yellowing resistant polyamide fiber structure of the present invention is treated with a gas phase acid anhydride, a gas phase and liquid phase acid anhydride, or a liquid phase acid anhydride.

The liquid acid anhydride is substantially 100% liquid acid anhydride, and does not include liquid acid anhydride.

By this acid anhydride treatment, it is possible to produce a yellowing-resistant polyamide fiber structure having good dyeability by blocking amino groups to the extent that dyeing properties are not affected.

The acid anhydride referred to in the present invention refers to a compound obtained by dehydration condensation of two acids, and a compound obtained by dehydration condensation of a divalent or higher valent acid in the molecule. Acetic anhydride, maleic anhydride, succinic anhydride, valeric anhydride, glutaric anhydride, benzoic anhydride, phthalic anhydride, hexanoic anhydride, naphthalic anhydride, trifluoroacetic anhydride, etc. can be used, but are not limited thereto. is not.

It is preferable to use acetic anhydride because it has a high vapor pressure at low temperatures, is inexpensive, and is highly safe.

The treatment with an acid anhydride is for covalently blocking the terminal amino group. Since it is blocked by covalent bond, unlike ionic bond, even when scouring or dyeing,
The yellowing prevention effect continues. In addition, by treating before scouring (raw machine), it is possible to prevent yellowing during storage and prevent yellowing before processing.

The treatment with a gas-phase acid anhydride or a liquid-phase acid anhydride blocks the terminal amino groups only in the fiber surface layer, so that the amino groups remaining in the dyeing seat, which are involved in dyeing inside the fiber, are removed. It can be blocked, and the dyeing property can be prevented.

On the other hand, in the solution treatment using a solution prepared by dissolving an acid anhydride in a solvent, even the amino groups in the fiber are blocked by the swelling effect of the solvent on the fiber, but there is an effect of preventing yellowing. Dyeability is significantly impaired.

In the case of treating with a liquid-phase acid anhydride, a dipping method, a spray method or the like can be used as the applying method. In the case of the dipping method, just dipping in an acid anhydride solution is effective,
The heating treatment may be performed in the immersed state or through a soaking / squeezing step.

In the case of the spray method, the acid anhydride may be applied by spraying, but heat treatment may be appropriately performed. For the heat treatment, various dyeing machines, ovens, pin tenters and the like can be used.

When the acid anhydride is treated in the gas phase, it is preferable to treat the acid anhydride at a vapor pressure of less than 760 mmHg, that is, a temperature of less than the boiling point. If the vapor pressure is higher than 0 mmHg at a temperature above the freezing point and below the boiling point, there is no difference in the effect of preventing yellowing depending on the temperature.

The polyamide fiber in the present invention means a fiber made of nylon 6, nylon 66, nylon 12, etc. The fibrous structure means a woven or knitted fabric, a non-woven fabric, cotton, or the like, but is not limited to this.

[0035]

EXAMPLES The present invention will now be described in more detail by way of examples.

Yellowing degree (ΔY) in Examples and Comparative Examples
I) was measured for undyed cloth and dyed cloth according to the following method.

The YI value was measured with a multi-light source spectrocolorimeter (Suga Test Instruments Co., Ltd.) with a C light source and a visual field of 2 °.

The color developability (L value) as an effect on the dyeability was also measured using the same measuring machine.

[Measurement of degree of yellowing (ΔYI)] 1. The YI value of the fabric is measured.

2. The cloth is immersed in a 0.5 wt% vanillin / ethanol solution, sandwiched between filter papers to absorb excess liquid, air-dried, and then heat-treated at 150 ° C. for 1 min.

3. The YI value of the fabric after the heat treatment is measured.

4. Subtract the YI value from the YI value to obtain Δ
YI. A yellow-resistant polyamide fiber structure having a ΔYI of less than 1 was used.

[Measurement of color developability (L value)] The following standard fabric specified in JIS L 0803 is dyed and the L value is measured.

Nylon taffeta Raw yarn: warp 70D, weft 70D Weave density: warp 214 yarns / 5 cm, weft 150 yarns / 5
cm Unit weight: 70 ± 5 g / m ² 2. The L value after dyeing the evaluation fabric is measured.

3. The L value was subtracted from the L value to obtain ΔL.

The dyeing conditions are as follows.

Dye: Kyanol Mill Black TL
R (Kayanol Mill Black TLR) Concentration: 5% owf Bath ratio: 1:20 Temperature x time: 98 ° C x 60 min pH: 4 (acetic acid adjustment) The fabrics used in Examples 1 to 10 and Comparative Examples 1 to 4 are as follows. It was manufactured by the method of.

[Cloth] Shrinkage rate of 9%, 50 by direct drawing method
A denier / 17 filament nylon 6 semi-dal yarn was spun and a tricot fabric was knitted by a warp knitting machine.

[Example 1] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth of the above cloth (15 cm x 10) was placed.
cm) was suspended in the flask. The flask was treated at 60 ° C. for 15 minutes. ΔYI and ΔL of the treated fabric and ΔYI after dyeing were determined. The evaluation results are shown in Table 1. Δ
YI is 0.4, ΔL is −4.2, and ΔYI after staining is 0.
It was 2, and a yellowing-resistant polyamide-based fiber structure having a high resistance to yellowing and having a natural appearance was obtained.

[0050]

[Table 1] [Example 2] 10 g of acetic anhydride was placed in a 2 L-separal flask, and the raw fabric (15 cm x 10 cm) of the above cloth was suspended in the flask. The flask was treated at 60 ° C. for 15 minutes. After the treatment, the cloth is sanded 29 (0.5g / l),
Refining was carried out for 20 minutes in an aqueous solution of Glauber's salt (0.5 g / l) at 60 ° C. The ΔYI and ΔL of the cloth after scouring and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 1. As shown in Table 1, ΔYI after scouring is 0.4, ΔL
Was -4.2, and ΔYI after dyeing was 0.2, and a yellowing-resistant polyamide fiber structure having good yellowing-preventing property even after scouring treatment and dyeing and having good dyeing property was obtained.

[Example 3] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth of the above cloth (15 cm x 10) was placed.
cm) was suspended in the flask. The flask is 140 ℃
For 3 minutes. After processing, the fabric is sanded 2
9 (0.5 g / l) and Glauber's salt (0.5 g / l) were dissolved in an aqueous solution at 60 ° C. for 20 minutes for scouring. ΔY of cloth after scouring
I and ΔL were determined. The evaluation results are also shown in Table 1. As shown in Table 1, ΔYI after scouring is 0.2, ΔL
Was -3.4, the ΔYI after dyeing was 0.1, and a yellowing-resistant polyamide fiber structure having a high yellowing-preventing property even after the scouring treatment and the dyeing and having a good dyeing property was obtained.

[Example 4] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth of the above cloth (15 cm x 10 cm) was added.
cm) was suspended in the flask. The flask was treated at 80 ° C. for 10 minutes. After treatment, rinse with hot water at 50 ° C for 12
It was dried at 0 ° C. for 2 minutes. ΔYI, ΔL of the dried cloth,
The ΔYI after dyeing was determined. The evaluation results are also shown in Table 1.

As shown in Table 1, ΔYI is 0.4, ΔL
Was -3.5 and the ΔYI after dyeing was 0.2, and a yellowing-resistant polyamide fiber structure having high yellowing-preventing property even after dyeing and good dyeability was obtained.

[Example 5] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth of the above cloth (15 cm x 10) was placed.
cm) was suspended in the flask. The flask was treated at 80 ° C. for 10 minutes. After processing, the fabric is sanded 29
(0.5 g / l) and Glauber's salt (0.5 g / l) were dissolved in an aqueous solution at 60 ° C. for 20 minutes for scouring. ΔYI of the cloth after scouring,
ΔL and ΔYI after dyeing were determined. The evaluation results are also shown in Table 1.

As shown in Table 1, ΔYI is 0.4, ΔL
Was -3.5, the ΔYI after dyeing was 0.2, and a yellowing-resistant polyamide fiber structure having good yellowing-preventing property even after scouring treatment and dyeing and having good dyeing property was obtained.

[Example 6] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth of the above cloth (15 cm x 10) was placed.
cm) was suspended in the flask. The flask is 100 ℃
Was processed for 3 minutes. After treatment, rinse with hot water at 50 ° C for 12
It was dried at 0 ° C. for 2 minutes. ΔYI, ΔL of the dried cloth,
The ΔYI after dyeing was determined. The evaluation results are also shown in Table 1.

As shown in Table 1, ΔYI is 0.2, ΔL
Was -3.8 and the ΔYI after dyeing was 0.1, and a yellowing-resistant polyamide fiber structure having a high yellowing-preventing property even after dyeing and having good dyeability was obtained.

[Example 7] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth of the above cloth (15 cm x 10) was placed.
cm) was suspended in the flask. The flask is 120 ℃
Was treated for 1 minute. After treatment, rinse with hot water at 50 ° C for 12
It was dried at 0 ° C. for 2 minutes. ΔYI, ΔL of the dried cloth,
The ΔYI after dyeing was determined. The evaluation results are also shown in Table 1.

As shown in Table 1, ΔYI is 0.2, ΔL
Was -3.8 and the ΔYI after dyeing was 0.1, and a yellowing-resistant polyamide fiber structure having a high yellowing-preventing property even after dyeing and having good dyeability was obtained.

[Example 8] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth of the above cloth (15 cm x 10 cm) was added.
cm) was suspended in the flask. The flask is 140 ℃
Was treated for 1 minute. After treatment, rinse with hot water at 50 ° C for 12
It was dried at 0 ° C. for 2 minutes. ΔYI, ΔL of the dried cloth,
The ΔYI after dyeing was determined. The evaluation results are also shown in Table 1.

As shown in Table 1, ΔYI is 0.2 and ΔL
Was -3.4, the ΔYI after dyeing was 0.1, and the yellowing-resistant polyamide-based fiber structure having high yellowing-preventing property even after dyeing and good dyeability was obtained.

[Example 9] 100 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth of the above cloth (15 cm x 1) was placed.
0 cm). The flask was treated at 60 ° C. for 10 minutes. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. ΔYI, ΔL of fabric after drying, Δ after dyeing
I asked for YI. The evaluation results are also shown in Table 1.

As shown in Table 1, ΔYI is 0.2 and ΔL
Was -3.8 and the ΔYI after dyeing was 0.1, and a yellowing-resistant polyamide fiber structure having a high yellowing-preventing property even after dyeing and having good dyeability was obtained.

[Example 10] The cloth (15 cm x 10 cm) was sprayed onto acetic anhydride so that the adhesion rate was 30%, and heat treatment was carried out at 140 ° C for 1 minute. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. The ΔYI and ΔL of the dried fabric and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 1.

As shown in Table 1, ΔYI is 0.2 and ΔL is
Was -3.4, the ΔYI after dyeing was 0.1, and the yellowing-resistant polyamide-based fiber structure having high yellowing-preventing property even after dyeing and good dyeability was obtained.

[Comparative Example 1] A raw fabric of the above cloth (15 cm x
10 cm) Sandette 29 (0.5 g / l), Glauber's salt (0.5 g / l)
Scouring was carried out for 20 minutes in a 60 ° C. aqueous solution in which 1) was dissolved. The ΔYI and ΔL of the cloth after scouring and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 1.

As shown in Table 1, ΔYI is 15.8, Δ
L was −4.4 and ΔYI after dyeing was 12.3, which was inferior in the yellowing prevention property because the acid anhydride treatment was not performed.

[Comparative Example 2] A raw fabric of the above cloth (15 cm x
10 cm) Sandette 29 (0.5 g / l), Glauber's salt (0.5 g / l)
Scouring was carried out for 20 minutes in a 60 ° C. aqueous solution in which 1) was dissolved. After scouring, it was treated under the following conditions with Y500 (manufactured by Yoshimura Kosan Co., Ltd.) which is an anti-yellowing agent, washed with hot water and air dried.

Treatment concentration = 1.5% owf Bath ratio = 1: 20 Treatment temperature × time = 95 ° C. × 30 min pH = 3 (acetic acid adjustment) After air drying, ΔYI, ΔL, and ΔYI after dyeing were determined. The evaluation results are also shown in Table 1.

Since yellowing was prevented by an ionic bond instead of acid anhydride treatment, the terminal amino group had a low blocking property, and dyeing further deteriorated the yellowing prevention property.

[Comparative Example 3] A raw fabric of the above cloth (15 cm x
10 cm) Sandette 29 (0.5 g / l), Glauber's salt (0.5 g / l)
Scouring was carried out for 20 minutes in a 60 ° C. aqueous solution in which 1) was dissolved. After scouring, it was immersed in a 2% methanol solution of acetic anhydride and treated at room temperature for 10 minutes. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. ΔY of dried cloth
I, ΔL, and ΔYI after staining were determined. The evaluation results are also shown in Table 1.

The dyeability was inferior due to the treatment with the acid anhydride solution.

[Comparative Example 4] A raw fabric of the above cloth (15 cm x
10 cm) Sandette 29 (0.5 g / l), Glauber's salt (0.5 g / l)
Scouring was carried out for 20 minutes in a 60 ° C. aqueous solution in which 1) was dissolved. After scouring, soak in a 1% aqueous solution of acetic anhydride to 40
It was treated at 0 ° C for 10 minutes. After treatment, rinse with hot water at 50 ° C for 12
It was dried at 0 ° C. for 2 minutes. ΔYI, ΔL of the dried cloth,
The ΔYI after dyeing was determined. The evaluation results are also shown in Table 1. The dyeability was inferior due to the treatment with the acid anhydride aqueous solution.

[Example 11] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth cloth (15 cm x 10 cm) specified in JIS L 0803 was suspended in the flask. The flask was treated at 60 ° C. for 15 minutes. ΔYI and ΔL of the treated fabric and ΔYI after dyeing were determined. The evaluation results are shown in Table 2. ΔYI is 0.4, Δ
L was 0.2 and ΔYI after dyeing was 0.2, and a yellowing-resistant polyamide fiber structure having a good yellowing resistance and having a natural yellowing resistance was obtained.

[0075]

[Table 2] [Example 12] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a raw fabric cloth (15 cm x 10 cm) defined in JIS L 0803 was suspended in the flask. The flask was treated at 60 ° C. for 15 minutes. After the treatment, the cloth is sanded 29 (0.5g / l), Glauber's salt (0.5g / l)
Scouring was carried out for 20 minutes in an aqueous solution of 60.degree. The ΔYI and ΔL of the cloth after scouring and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 2. As shown in Table 2, ΔYI after scouring is 0.4, ΔL is 0.2, and ΔYI after dyeing is 0.2, which shows high yellowing-preventing property even after scouring treatment and dyeing and good dyeability. A yellowing resistant polyamide fiber structure was obtained.

[Example 13] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth cloth (15 cm x 10 cm) specified in JIS L 0803 was suspended in the flask. The flask was treated at 140 ° C. for 3 minutes. After the treatment, the cloth was scoured in an aqueous solution of Sandet 29 (0.5 g / l) and Glauber's salt (0.5 g / l) at 60 ° C. for 20 minutes. The ΔYI and ΔL of the cloth after scouring were determined.
The evaluation results are also shown in Table 2. As shown in Table 2, ΔYI after scouring is 0.2, ΔL is 1.0, and ΔYI after dyeing is 0.1, which shows high yellowing-preventing property even after scouring treatment and dyeing and good dyeability. A yellowing resistant polyamide fiber structure was obtained.

[Example 14] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth raw fabric (15 cm x 10 cm) specified in JIS L 0803 was suspended in the flask. The flask was treated at 80 ° C. for 10 minutes. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. The ΔYI and ΔL of the dried fabric and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 2.

As shown in Table 2, ΔYI is 0.4, ΔL
Was 0.9 and the ΔYI after dyeing was 0.2, and a yellowing-resistant polyamide fiber structure having high yellowing-preventing property even after dyeing and good dyeability was obtained.

[Example 15] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth cloth (15 cm x 10 cm) defined in JIS L 0803 was suspended in the flask. The flask was treated at 80 ° C. for 10 minutes. After the treatment, the fabric was scoured for 20 minutes in an aqueous solution of Sandet 29 (0.5 g / l) and Glauber's salt (0.5 g / l) at 60 ° C. ΔYI, ΔL of cloth after scouring, Δ after dyeing
I asked for YI. The evaluation results are also shown in Table 2.

As shown in Table 2, ΔYI is 0.4, ΔL
Of 0.9 and ΔYI of 0.2 after dyeing,
A yellowing-resistant polyamide-based fiber structure having a high yellowing-preventing property even after dyeing and having a good dyeing property was obtained.

[Example 16] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth cloth (15 cm x 10 cm) specified in JIS L 0803 was suspended in the flask. The flask was treated at 100 ° C. for 3 minutes. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. The ΔYI and ΔL of the dried fabric and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 2.

As shown in Table 2, ΔYI is 0.2, ΔL
Was 0.6 and the ΔYI after dyeing was 0.1, and a yellowing-resistant polyamide fiber structure having high yellowing-preventing property even after dyeing and good dyeability was obtained.

[Example 17] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth fabric (15 cm x 10 cm) specified in JIS L 0803 was suspended in the flask. The flask was treated at 120 ° C. for 1 minute. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. The ΔYI and ΔL of the dried fabric and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 2.

As shown in Table 2, ΔYI is 0.2 and ΔL
Was 0.6 and the ΔYI after dyeing was 0.1, and a yellowing-resistant polyamide fiber structure having high yellowing-preventing property even after dyeing and good dyeability was obtained.

[Example 18] 10 g of acetic anhydride was placed in a 2 L-separal flask, and a cloth cloth (15 cm x 10 cm) defined in JIS L 0803 was suspended in the flask. The flask was treated at 140 ° C. for 1 minute. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. The ΔYI and ΔL of the dried fabric and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 2.

As shown in Table 2, ΔYI is 0.2 and ΔL
Was 1.0 and the ΔYI after dyeing was 0.1, and a yellowing-resistant polyamide fiber structure having a high yellowing-preventing property even after dyeing and having good dyeability was obtained.

Example 19 100 g of acetic anhydride was added to 2 L-
The cloth is placed in a separal flask and a cloth cloth (15 cm × 10 cm) defined in JIS L 0803 is immersed therein. The flask was treated at 60 ° C. for 10 minutes. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. The ΔYI and ΔL of the dried fabric and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 2.

As shown in Table 2, ΔYI is 0.2 and ΔL
Was 0.6 and the ΔYI after dyeing was 0.1, and a yellowing-resistant polyamide fiber structure having high yellowing-preventing property even after dyeing and good dyeability was obtained.

[Example 20] Spraying was carried out on a cloth cloth (15 cm x 10 cm) specified in JIS L 0803 so that acetic anhydride had an adhesion rate of 30%, and then 140
Heat treatment was performed at 1 ° C. for 1 minute. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. ΔY of dried cloth
I, ΔL, and ΔYI after staining were determined. The evaluation results are also shown in Table 2.

As shown in Table 2, ΔYI is 0.2 and ΔL
Was 1.0 and the ΔYI after dyeing was 0.1, and a yellowing-resistant polyamide fiber structure having a high yellowing-preventing property even after dyeing and having good dyeability was obtained.

Comparative Example 5 Sandet 29 (0.5 g / l) and Glauber's salt (0.5 g / l) were melted at 60 ° C. in a cloth cloth (15 cm × 10 cm) specified in JIS L 0803.
Scouring was performed for 20 minutes in the aqueous solution of The ΔYI of the cloth after scouring and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 2.

As shown in Table 2, ΔYI was 15.8 and ΔYI after dyeing was 12.3, which was inferior in the yellowing preventive property because the acid anhydride treatment was not performed.

[Comparative Example 6] Sandet 29 (0.5 g / l) and mirabilite (0.5 g / l) were melted at 60 ° C. into a cloth cloth (15 cm × 10 cm) specified in JIS L 0803.
Scouring was carried out for 20 minutes in the above aqueous solution. After scouring, it was treated under the following conditions with Y500 (manufactured by Yoshimura Kosan Co., Ltd.) which is an anti-yellowing agent, washed with hot water and air dried.

Treatment concentration = 1.5% owf Bath ratio = 1: 20 Treatment temperature × time = 95 ° C. × 30 min pH = 3 (acetic acid adjustment) After air drying, ΔYI, ΔL, and ΔYI after dyeing were determined. The evaluation results are also shown in Table 2.

Since yellowing was prevented by an ionic bond rather than by acid anhydride treatment, the terminal amino group had a low blocking property, and dyeing resulted in a further inferior yellowing resistance.

[Comparative Example 7] Sandet 29 (0.5 g / l) and mirabilite (0.5 g / l) were melted at 60 ° C. in a cloth cloth (15 cm × 10 cm) specified in JIS L 0803.
Scouring was carried out for 20 minutes in the above aqueous solution. After scouring, it was immersed in a 2% methanol solution of acetic anhydride and treated at room temperature for 10 minutes. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. The ΔYI and ΔL of the dried fabric and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 2.

The dyeability was inferior due to the treatment with the acid anhydride solution.

[Comparative Example 8] Sandet 29 (0.5 g / l) and mirabilite (0.5 g / l) were melted at 60 ° C. into a cloth cloth (15 cm × 10 cm) specified in JIS L 0803.
Scouring was carried out for 20 minutes in the above aqueous solution. After scouring, it was immersed in a 1% aqueous solution of acetic anhydride and treated at 40 ° C. for 10 minutes. After the treatment, it was washed with hot water at 50 ° C and dried at 120 ° C for 2 minutes. The ΔYI and ΔL of the dried fabric and the ΔYI after dyeing were determined. The evaluation results are also shown in Table 2. The dyeability was inferior due to the treatment with the acid anhydride aqueous solution.

[0099]

EFFECT OF THE INVENTION The yellowing resistant polyamide fiber structure of the present invention has an excellent effect of preventing yellowing and also has excellent durability.

According to the method of the present invention, the polyamide-based fiber structure can be easily post-processed for yellowing resistance even in a raw machine, and it is effective for yellowing during storage, and the effect is maintained even after scouring and dyeing. It does not affect the dyeing. Moreover, the process safety is high, and it is possible to manufacture at low cost.
It can be applied to all polyamide fibers.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Jiro Amano 1-1-1, Sonoyama, Otsu City, Shiga Toray Co., Ltd. Shiga Business Office

Claims (4)

[Claims] 1. A yellowing-resistant polyamide fiber structure, wherein the yellowing of the polyamide fiber structure due to vanillin is ΔYI <1. 2. The yellowing-resistant polyamide-based fiber structure according to claim 1, wherein the coloring property by dyeing is −5 <ΔL <5. 3. A method for producing a yellowing-resistant polyamide-based fiber structure, which comprises treating the polyamide-based fiber structure with a gas phase and / or a liquid phase of an acid anhydride. 4. The method for producing a yellowing-resistant polyamide-based fiber structure according to claim 3, wherein the acid anhydride is acetic anhydride.