JP2000256959A - Caustic reduction method for polyester-based fabric - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a caustic reduction method for polyester-based fiber fabrics, excellent in effects for removing monomers and oligomers and capable of certain ly presenting caustic reduction products of high quality. SOLUTION: This caustic reduction method for polyester-based fibers of the invention is specific to treat a polyester-based fabric to reduce its weight in 5-50 wt.% by using a caustic reduction agent comprising an activation agent containing a sulfonated compound of a polyoxyethylene styrylphenyl ether expressed by the formula [X is H, K, Na, Li or quaternary ammonium; (n1) is 10-20; (n2) is 2-5], a carboxyl group-containing polymer and/or a salt of carboxyl-containing polymer and 0.5-6 wt.% alkali.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a method for reducing the weight of a polyester fiber cloth, which has an excellent effect of removing monomers and oligomers and can provide a high-quality processed product.

[0002]

2. Description of the Related Art When treating fiber products such as polyester fibers or fabrics containing polyester fibers, minute impurities such as oligomers are generated, and these may cause processing defects such as uneven dyeing. Are known. As a technique for removing these impurities, the present inventors have used a fiber treating agent comprising a cationic organic compound, a nonionic anion activator, a polymer containing a carboxyl group, and the like,
Japanese Patent Laid-Open No. 8-1 discloses a method for treating a polyester fiber product.
It has been previously proposed in Japanese Patent Publication No. 13873. But,
Although this method shows an oligomer removing effect superior to the conventional method, there is a problem that a sufficient oligomer dispersing effect cannot be obtained, a long time treatment is required, and the cost is increased.

[0003]

SUMMARY OF THE INVENTION In view of the above-mentioned problems of the prior art, the present invention provides a method for reducing the weight of a polyester fiber cloth, which has an excellent effect of removing monomers and oligomers and reliably provides a high-quality processed product. Is to be provided.

[0004]

The present invention employs the following means in order to solve the above-mentioned problems. That is, the method for reducing the weight of a polyester fiber fabric according to the present invention comprises an activator containing a sulfonated polyoxyethylene styryl phenyl ether represented by the following general formula [I], a carboxyl group-containing polymer and / or a salt of a carboxyl group. Containing polymer, 0.5 to 6% by weight
The polyester-based fiber cloth is subjected to a weight-reduction treatment of 5 to 50% by weight using a weight-reducing agent containing an alkali.

[0005]

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Wherein n ₁ : 10 to 20 n ₂ : 2 to 5 X: H, K, Na, Li or quaternary ammonium

[0007]

DETAILED DESCRIPTION OF THE INVENTION The present invention has been made to solve the above-mentioned problems, namely,
We thoroughly studied the method of reducing the weight of polyester fiber cloth that excels in removing monomers and oligomers and reliably provides high-quality weight-loss processed products. It was determined that it could be solved.

[0008] Such a weight loss treatment agent is a treatment agent comprising an activator containing a sulfonated product of polyoxyethylene styryl phenyl ether, a carboxyl group-containing polymer and / or a salt-containing polymer of a carboxyl group, and an alkali. .

The anion activator containing a sulfonated polyoxyethylene styryl phenyl ether includes an activator containing a sulfonated polyoxyethylene styryl phenyl ether represented by the following general formula [I]. This activator has a function of dispersing the oligomer and preventing insolubilization.

[0010]

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However, n ₁ : 10 to 20 n ₂ : 2 to 5 X: H, K, Na, Li or quaternary ammonium In the general formula [I], when n ₁ exceeds 20, the dispersibility becomes large. However, foaming also increases, causing trouble during processing. If it is less than 10, foaming is suppressed, but the dispersibility tends to decrease. Also,
n ₂ is good to use a range of 2 to 5 in order to impart hydrophobicity to the oligomer.

Further, since the compound represented by the general formula [I] is sulfonated, it has excellent heat resistance, and has a characteristic that a stable oligomer dispersion effect can be obtained even in the simultaneous dyeing treatment.

Next, the weight-reducing agent of the present invention contains the above-mentioned activator and further contains the carboxyl group-containing polymer, the carboxyl group salt-containing polymer, or both. These polymers have a function of stably dispersing the insolubilized oligomer and preventing re-attachment to the fabric.

As such a polymer, (CH ₂ C
H ₂₎ in the polymer main chain represented by n, a carboxyl group (-COOH) and sodium carboxylate groups (-
COONa) is bonded as a side chain, and specifically, for example, an acrylic acid polymer, a methacrylic acid polymer or a salt thereof can be used. Among such polymers, the molecular weight is 1,000 to 20,000
Those in the range are particularly preferably used.

The mixing ratio of the activator (A) and the carboxyl group-containing polymer and / or the carboxyl group salt-containing polymer (B) is expressed by the weight ratio (A / B) with respect to the polymer 1 of (B) and (A). ) Is preferably used in a proportion of 3 to 6 in order to improve the dispersion stability of the oligomer in the aqueous alkali solution. Even if the ratio of (A) is too high outside the above range,
The effect of removing the oligomer reaches saturation, and it does not make sense to add more, but if it is too low, the effect of removing the oligomer tends to decrease.

The weight-reducing agent of the present invention is used for reducing the weight of a polyester fiber cloth. Examples of the polyester fiber include polyethylene terephthalate, polybutylene terephthalate and a copolymer thereof. Polyester-based fibers can be used. As a form of such a fiber, either a short fiber or a long fiber may be used. Examples of the fiber cloth containing such polyester fibers include blended yarns, composite yarns, blended yarns, mixed knits, mixed weaves, and mixed nonwoven fabrics of polyester fibers and other natural fibers or synthetic fibers. Above all, the processing effect of the present invention is greatly reflected in a polyester fiber cloth made of a fiber composed of a polymer having a structure in which oligomers are easily generated.

Next, a method for reducing weight using the agent for reducing weight of the present invention will be described. For such a weight reduction treatment, the aforementioned weight reduction treatment agent, specifically, a treatment agent composed of a mixed aqueous solution of the above (A) and (B) and an alkali is used. As the alkali, any alkaline substance such as caustic soda and soda ash may be used, but caustic soda is preferably used because it has a large effect. The concentration of the reducing agent is preferably 1 to 5 g, more preferably 2 to 4 g, per liter of the aqueous solution. The aqueous solution here includes a dyeing solution and other systems containing a processing agent.

The weight reduction treatment temperature of the present invention is preferably 40
Although it may be in the range of 120 to 120 ° C., considering the various physical properties and texture of the polyester fiber cloth, 80 to 100 ° C.
Is preferable. Such weight reduction treatment may be performed before, during, or after staining.

[0019]

The present invention will be described below in more detail with reference to examples. In addition, the measurement of the oligomer adhesion amount after the treatment in the examples is performed by extracting the fiber surface oligomer of 1 g of the fiber cloth using methanol, drying the extract, dissolving the solid matter in chloroform, and using liquid chromatography. , Measuring the amount of trimers and tetramers of the polyester,
It was defined as the amount of adhesion.

The visual judgment was carried out by taking an image using a scanning electron microscope to check the adhesion of oligomers present on the surface of the fiber cloth, and evaluated the following four steps.

◎: There is no oligomer on the fiber surface ○: Slightly adhered to the fiber surface △: Sparsely adhered to the fiber surface ×: Adhered to the entire fiber surface For foaming, during processing
It was evaluated visually with the following three grades.

：: Almost no bubbling △: A little bubbling ×: A lot of bubbling The following weight loss treatment agent is dyed on plain woven fabric (warp yarn density: 110 yarns per inch, weft yarn density: 80 yarns per inch) in a dyeing bath before heating in a dyeing process using a liquid jet dyeing machine. 2.0 g was added per liter of the solution, and a usual simultaneous dyeing and reduction treatment at 130 ° C. was performed. Next, the woven fabric was washed with hot water in a usual manner, spread, dried at 130 ° C., and finished.

The weight-reducing agent is represented by the following general formula:
Polyoxyethylene styryl phenol ether sulfonate (n ₁ = 15, n) which is an activator represented by [I]
₂ = 4, X = Na) (A) and a mixture of a carboxyl group-containing polymer (B) and an acrylic acid polymer having a molecular weight of 10000, in a weight ratio (A / B) of 4: 1 in the above order.
And used at a ratio of

[0024]

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During the weight reduction treatment, there was no problem due to foaming, and the oligomer adhesion amount of the woven fabric after processing was measured to be 490 ppm. In addition, the adhesion of the oligomer to the fiber surface was slight even by visual inspection using an electron microscope, and the obtained woven fabric was of excellent quality without defects due to the adhesion of the oligomer. Comparative Example 1 Same as Example 1 except that a mixture of the activator represented by the general formula [I] and the carboxyl group-containing polymer acrylic acid polymer was not used in the same polyester plain fabric used in Example 1. And subjected to a finishing process.

The woven fabric obtained was 1110 ppm when the oligomer adhesion amount was measured. In addition, in the naked eye judgment by an electron microscope, the oligomer was attached to the entire fiber surface, and the quality was rejected. Comparative Example 2 Using the same polyester plain woven fabric as used in Example 1,
As a weight-reducing agent, unlike Example 1, a cationic organic compound octylpicolinium chloride (C ₁₄ H ₂₄
N ⁺ Cl ⁻ ), a nonionic surfactant of polyoxyethylene styryl phenyl ether and an anionic surfactant of sodium sulfonate of polyoxyethylene styryl phenyl ether, and a carboxyl group-containing polymer having a molecular weight of 80,000 acrylic acid polymer. Except for compounding, the same addition as in Example 1 was carried out, the dyeing was simultaneously reduced, washed with hot water, spread, dried and finished.

During the weight loss treatment, foaming was large, and the oligomer adhesion amount after processing was measured to be 990 ppm. In addition, in the naked eye judgment by an electron microscope, the oligomer was attached to the entire fiber surface, and the quality was rejected. Example 2 Using the same polyester plain fabric as used in Example 1,
Furthermore, after performing normal dyeing at a dyeing temperature of 130 ° C. using a liquid jet dyeing machine, the temperature was lowered. During the cooling, the temperature was kept constant at 80 ° C., and a weight-loss treatment agent having the same composition as that used in Example 1 was added and blended in the dyeing bath in the same ratio. At this time, 2.0 g of the reducing agent was used per liter of the staining solution.
And NaOH (30% aqueous solution) at a ratio of 4.0 g were added to the dye bath, and the dyed fabric was subjected to a weight reduction treatment for another 20 minutes. After this weight reduction treatment, the woven fabric was washed with hot water, spread, and dried at 130 ° C. for finishing in a usual manner.

During the weight loss treatment, there was almost no bubbling,
When the amount of oligomer attached to the woven fabric was measured, it was 270 p.
pm. In the case of visual inspection using an electron microscope,
There is almost no adhesion of oligomer on the fiber surface, and the obtained woven fabric
Has no defects due to oligomer adhesion and has excellent quality.
Was. Comparative Example 3 On the same polyester plain fabric as used in Example 2,
Instead of the weight loss treatment agent of Example 2, a cationic organic compound
Octyl picolinium chloride (C₁₄H_{twenty four}N ⁺C
l^-) And the nonionic activator polyoxyethylene styryl
Phenyl ether and anionic surfactant polyoxye
Sodium sulfonate of tylenestyril phenyl ether
And carboxyl group-containing polymers having a molecular weight of 8
A mixture with 0000 acrylic acid polymer and NaOH
(30% aqueous solution) in a dye bath as in Example 2,
Except for blending, a weight loss treatment was performed in the same manner as in Example 2,
Wash the treated fabric with hot water, spread it at 130 ℃
It was dried and finished.

During the weight loss treatment, the foaming was large and the running of the fabric was unstable, but the amount of oligomer adhered to the woven fabric after processing was measured to be 330 ppm. In addition, in the naked eye judgment by an electron microscope, the resulting fabric had almost no adhesion of the oligomer to the fiber surface, and the obtained woven fabric showed no defect due to the oligomer, but was rejected due to physical defects such as blurred eyes.

The processing results of Examples 1 and 2 and Comparative Examples 1 to 3 are summarized in Table 1.

[0031]

[Table 1]

[0032]

According to the present invention, it is possible to provide a polyester fiber cloth in the form of a good-quality cloth having no weight loss processing defects, and to carry out such a weight loss treatment without running trouble due to bubbles. In addition, there is an advantage that the dyeing can be simultaneously reduced, and the time can be reduced and the process can be simplified.

Claims (3)

[Claims] 1. An activator containing a sulfonated polyoxyethylene styryl phenyl ether represented by the following general formula [I], a carboxyl group-containing polymer and / or a carboxyl group salt-containing polymer, and 0.5 to 6% by weight. %
A weight reduction treatment of a polyester fiber cloth, wherein the polyester fiber cloth is subjected to a weight reduction treatment of 5 to 50% by weight using a weight loss treatment agent containing an alkali. Embedded image Where n ₁ : 10 to 20 n ₂ : 2 to 5 X: H, K, Na, Li or quaternary ammonium 2. The weight ratio (A / B) of the activator (A) and the carboxyl group-containing polymer and / or the carboxyl group-containing polymer (B) is 3 to 6: 1. 2. The method for reducing the weight of a polyester fiber cloth according to item 1. 3. The method according to claim 1, wherein the carboxyl group-containing polymer or the carboxyl group salt-containing polymer is 1,000 to 20,000.
The method for weight-reducing a polyester fiber cloth according to claim 1 or 2, which has a molecular weight of: