JPH09195160A - Production of modified cellulose acetate fiber - Google Patents

Abstract

PROBLEM TO BE SOLVED: To shorten an enzymatic treatment time in a softening treatment of an acetate fiber comprising carrying out an alkali treatment of an acetate fiber and treatment with a cellulose decomposition enzyme. SOLUTION: Acetate fiber alone or a conjugate yarn comprising the acetate fiber and other fiber is subjected to alkali treatment with an alkali compound to convert at least surface of cellulose acetate fiber to cellulose. Then, the treated conjugate yarn is subjected to enzymatic treatment with a cellulolytic enzyme to decompose and remove the cellulose-forming part. In the alkali treatment by the alkali compound, the alkali treatment is carried out by jointly using hydrogen peroxide and a quaternary ammonium salt together with the alkali compound.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a method for producing a modified cellulose acetate fiber.

[0002]

2. Description of the Related Art Conventionally, a method for reducing the weight of cellulosic natural fibers by enzyme treatment to improve the smooth and soft texture of the fiber surface and to improve the hygroscopicity has been disclosed in Japanese Examined Patent Publication No. 52- It is disclosed and known in Japanese Patent No. 48236. Regarding the cellulose acetate fiber, there is no enzyme that directly acts industrially, and it was difficult to apply the same enzyme treatment as that of the cellulosic natural fiber, but the present applicants controlled the surface of the cellulose acetate fiber. As a method of decomposing with good properties, JP-A-5-2720
Japanese Patent Application Laid-Open No. 7-
Japanese Patent No. 26471 proposes a method of shortening the enzyme treatment time by adding a quaternary ammonium salt during alkali treatment.

[0003]

SUMMARY OF THE INVENTION An object of the present invention is to improve the method proposed in Japanese Patent Laid-Open No. 5-272067 and Japanese Patent Laid-Open No. 7-26471 to improve the enzyme treatment time. It is to provide a method for producing a cellulose acetate fiber.

[0004]

The gist of the present invention is to treat at least the surface of cellulose acetate fibers by subjecting cellulose acetate fibers alone or a composite yarn composed of cellulose acetate fibers and other fibers to alkali treatment with an alkali compound. Of the modified cellulose acetate fiber, which is characterized by carrying out alkali treatment in combination with hydrogen peroxide during alkali treatment with an alkali compound when decomposing and removing the cellulosic portion by enzymatic treatment with cellulose decomposing enzyme. It is a manufacturing method.

The cellulose acetate fiber used in the present invention may be cellulose triacetate having an acetylation degree of 56.2% to 62.5% or cellulose diacetate having an acetylation degree of 48.8% to 56.2%. The shape may be either filament or staple.

In the present invention, the cellulose acetate fiber or the composite yarn composed of the cellulose acetate fiber and other fibers is treated with a treating agent comprising an alkali compound and hydrogen peroxide, and optionally a quaternary ammonium salt in combination. Then, at least the surface of the cellulose acetate fiber is made to be cellulose, and the cellulose itself is mainly due to the action of the alkali compound, but when hydrogen peroxide is used in combination with the alkali compound (the quaternary ammonium salt may be When used in combination with addition), the weight loss rate can be greatly improved in the subsequent enzyme treatment, which gives good results.

Examples of the alkali compound used in the present invention include alkali metal hydroxides such as sodium hydroxide and potassium hydroxide, alkaline earth metal hydroxides such as calcium hydroxide and magnesium hydroxide, sodium hydrogen carbonate and carbonic acid. Examples thereof include conjugate salts of a strong alkali such as sodium and a weak acid.

Further, the hydrogen peroxide used in the present invention may be one generally used in the step of exposing cotton products, and examples thereof include industrial preparations (30 to 35% by weight).

Further, as the quaternary ammonium salt which is optionally used in the present invention, DYK-1125, DX
Y-10N (above, one company), Marserine PES, Marserin PEL, Mercerin PEF (above, Meisei Chemical Co., Ltd.), Catiosol NS-11conc (Takamatsu Yushi Co., Ltd.), Neolate NCB (Nikaka Chemical Co., Ltd.) Manufactured by KK), Silfine PE (manufactured by Senka Co., Ltd.), etc.

In order to obtain the modified cellulose acetate fiber of the present invention, the cellulose acetate fiber is used in an amount of 0.5 to 40% by weight of an alkali compound (based on cellulose acetate fiber) and a hydrogen peroxide solution of 0.5 to 15 g / l. Alkali treatment by immersing in a treatment agent consisting of (35% by weight aqueous solution), and optionally a treatment agent in which 0.5 to 12 g / l of a quaternary ammonium salt is used in combination at room temperature to 130 ° C. for 5 to 120 minutes. To do. By the alkali treatment, at least the surface of the cellulose is converted to cellulose acetate fibers, and the cellulose layer is decomposed and removed by enzymatic treatment with a cellulolytic enzyme.

The cellulolytic enzymes used in the present invention include those of filamentous fungi such as Trichoderma sp., Aspergillus sp. It is easily available under the trade name of (Novo). 1 to 50 g / l of these cellulolytic enzyme preparations, pH 3.5 to 7
The cellulosic layer of the cellulose acetate fiber can be decomposed and removed by immersing in the aqueous solution of 20 to 65 ° C. for 2 to 120 minutes.

In the modified cellulose acetate fiber of the present invention, the surface layer portion of the fiber may be cellulosized, that is, the base cellulose acetate fiber, and the surface layer portion may be a cellulosic layer, The greater the amount of the modified layer removed and reduced by the amount of the enzyme, the more preferable it is because the basic performance of the cellulose acetate fiber can be maintained and the texture is softened.

In the alkali treatment of the present invention, the selection, concentration, temperature, time, etc. of the alkali compound are adjusted according to the degree of modification of the modified cellulose acetate fiber.
In the enzyme treatment, the treatment time and the like are adjusted depending on the amount of the cellulosic portion.

The cellulose acetate fiber in the present invention can be made into a composite yarn by being combined with one or more kinds of other fibers, and the other fibers to be combined are natural fibers such as silk and wool. Examples of the fibers include chemical fibers such as fibers, nylon fibers, polyester fibers, acrylic fibers, polyurethane fibers, and the shape thereof may be filaments or staples. Further, as the compounding method, any known method such as air compounding, compound false twisting, and false twisting can be applied.

The modified cellulose acetate fiber composite yarn of the present invention can be obtained basically by the same method as in the case of the modified cellulose acetate fiber described above. Accordingly, the alkaline treatment conditions and the enzyme treatment conditions are appropriately changed within the range of the above conditions.

The applicant of the present invention, by adding a quaternary ammonium salt to an alkali compound and treating it as proposed in JP-A-7-26471, compared with the case of using only the alkali compound, the enzyme treatment of cellulose acetate fiber. It has been found that the speed of weight loss can be greatly improved. Further, in the present invention, hydrogen peroxide can be further improved by adding hydrogen peroxide instead of or in addition to the alkaline compound and the quaternary ammonium salt. The reason for this is not clear, but the cellulose formed by adding hydrogen peroxide during the alkaline treatment is structurally loosened more than the conventional one, and the treatment solution of the cellulolytic enzyme is more likely to penetrate. It is thought that

[0017]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The details of the present invention will be described below.
To obtain the cellulose acetate fiber used in the present invention,
The following method is adopted. Flake of cellulose triacetate or cellulose diacetate was dissolved in a single solvent such as methylene chloride or acetone or a mixed solvent such as methylene chloride and methanol to prepare a stock solution having a solution concentration of 15 to 30% by weight, preferably 18 to 27% by weight. Prepare.

In this way, the spinning dope is supplied to the spinning nozzle device and spun by the dry spinning method in which it is discharged into a high temperature atmosphere. Note that wet spinning may be performed instead of dry spinning.

The cellulose acetate fiber thus obtained is formed into a cloth. In the fiber state, that is, in the plastic bobbin winding state or the skein winding state, the following alkali treatment with an alkali compound and enzyme treatment may be performed, but industrially, it is preferable to perform weaving and knitting before performing the treatment.

Generally, after the fabric is formed, it is scoured and dried, and the scoured fabric is treated with a treating agent consisting of an alkali compound and hydrogen peroxide, and optionally a quaternary ammonium salt in combination, to give a cellulose acetate fiber. Of at least the surface of. Next, this cloth is dipped in an aqueous solution of a cellulolytic enzyme, washed with water and dried to obtain a cloth made of the modified cellulose acetate fiber of the present invention.

[0021]

The present invention will be described below in more detail with reference to examples. The evaluation in the examples was based on the following method.

(Enzyme treatment weight loss rate): [(Weight of fabric before enzyme treatment-Weight of fabric after enzyme treatment) / Weight of fabric before enzyme treatment] × 100 (%)

(Soft feeling): judged by handling in comparison with the fabric before enzyme treatment ◎: good × no change

Examples 1 and 2 Bright 75d / 2 made of cellulose triacetate fiber having an acetylation degree of 61.3%
Five satin weaves (warp density of 200 yarns / inch, weft density of 87 yarns / inch) using 0f as warps and Bright 100d / 26f as wefts were scoured and dried in a 6-tank continuous scouring machine. 7% by weight of sodium hydroxide having a bath ratio of 1:20 (vs. woven fabric), 2 g / l of quaternary ammonium salt, Mercerin PEF (manufactured by Meisei Chemical Co., Ltd.), and hydrogen peroxide (35% by weight aqueous solution) were added to the scoured woven fabric. Was added to an aqueous solution containing 5 g / l,
The temperature was raised from 30 ° C. to 2 ° C./min, and alkali treatment was performed at 120 ° C. for 60 minutes to make the fiber surface of the constituent fibers cellulose, and an alkali-treated woven fabric with an alkali weight loss rate of 7.2% was obtained. Next, this woven fabric was made into Cellsoft (Novo Cellulose Degrading Enzyme Preparation) 5 g / l, Bio-Assist MT (Moriroku Corporation) 5
It was immersed in an aqueous solution containing g / l at pH 4.8, 53 ° C. and a bath ratio of 1:50, and was treated with enzyme for 30 minutes and 60 minutes while stirring, washed with water and dried. The enzyme treatment weight loss rate and softness of the obtained woven fabric were evaluated, and the evaluation results are shown in Table 1.

(Comparative Examples 1 and 2) The same refined fabric as in Examples 1 and 2 was treated with 7% by weight of sodium hydroxide having a bath ratio of 1:20 (based on fabric) and quaternary ammonium salt, merceline PEF.
(Manufactured by Meisei Chemical Co., Ltd.) was added to an aqueous solution containing 2 g / l, and 30
The temperature was raised from 2 ° C./minute to 2 ° C./minute, and alkali treatment was carried out at 120 ° C. for 60 minutes to give cellulose fibers on the fiber surface of the constituent fibers to obtain an alkali-treated woven fabric with an alkali weight loss rate of 7.2%. Then
This woven fabric was subjected to enzyme treatment and evaluation under the same conditions as in Examples 1 and 2, and the evaluation results are shown in Table 1.

[0026]

[Table 1]

(Examples 3 to 4) An air-entangled composite yarn of cellulose triacetate fiber bright 75d / 20f having a degree of acetylation of 61.3% and polyester fiber semidull 20d / 12f, and a 5-sheet satin fabric used for warp and weft ( Density 160
(6 lines / inch, weft density 70 lines / inch) were scoured and dried in a 6-tank continuous scouring machine. 5.5% by weight of sodium hydroxide having a bath ratio of 1:20 (based on the woven fabric) and 2 g of quaternary ammonium salt, Mercerin PEF (manufactured by Meisei Chemical Co., Ltd.) were added to the scoured fabric.
/ L and hydrogen peroxide (35 wt% aqueous solution) were added to an aqueous solution containing 5 g / l, and the temperature was raised from 30 ° C to 2 ° C / min.
Alkali treatment was performed at 60 ° C. for 60 minutes to make the fiber surface of the constituent fibers cellulose, and an alkali-treated woven fabric with an alkali weight loss rate of 5.7% was obtained. Next, this woven fabric contains Cellsoft (a cellulose degrading enzyme preparation manufactured by Novo Co., Ltd.) 5 g / l, Bio Assist MT (manufactured by Moriroku Co., Ltd.) 5 g / l, pH 4.8, 53 ° C.,
Dipping in an aqueous solution with a bath ratio of 1:50 and stirring for 30 minutes, 6
It was treated with an enzyme for 0 minutes, washed with water and dried. The enzyme treatment weight loss rate and softness of the obtained woven fabric were evaluated, and the evaluation results are shown in Table 2.

(Comparative Examples 3 to 4) The same scouring fabric as in Examples 3 to 4 was added with 5.5% by weight of sodium hydroxide having a bath ratio of 1:20.
(Against fabric) and quaternary ammonium salt mercerin PE
F (manufactured by Meisei Chemical Co., Ltd.) was added to an aqueous solution containing 2 g / l, and 3
The temperature was raised from 0 ° C. to 2 ° C./min, and alkali treatment was performed at 120 ° C. for 60 minutes to make the fiber surface of the constituent fibers cellulose, and an alkali-treated woven fabric with an alkali weight loss rate of 5.8% was obtained. Next, this woven fabric was subjected to enzyme treatment and evaluation under the same conditions as in Examples 3 to 4, and the evaluation results are shown in Table 2.

[0029]

[Table 2]

[0030]

EFFECTS OF THE INVENTION According to the present invention, cellulose acetate fibers and composite yarns composed of cellulose acetate fibers and other fibers are treated with a treating agent containing an alkali compound, a quaternary ammonium salt and hydrogen peroxide, and then treated with an enzyme. As a result, the rate of enzyme weight loss is improved as compared with the conventional method, and thus modified cellulose acetate fiber and modified cellulose acetate fiber composite yarn having a soft texture can be efficiently obtained.

Claims (2)

[Claims] 1. A cellulose acetate fiber alone or a composite yarn comprising a cellulose acetate fiber and another fiber is alkali-treated with an alkali compound to make at least the surface of the cellulose acetate fiber cellulose, and then enzymatically treated with a cellulolytic enzyme. A method for producing a modified cellulose acetate fiber, characterized in that, when the celluloseized portion is decomposed and removed, hydrogen peroxide is used together with the alkali compound for alkali treatment. 2. The method for producing a modified cellulose acetate fiber according to claim 1, wherein a quaternary ammonium salt is used together with the alkali treatment with an alkali compound.