JPH09158043A - Fiber structure and its production - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a cellulosic fiber structure, having the shape stability and a soft touch feeling and useful for undershirt fabrics, etc., by carrying out the weight reduction treatment of a cellulosic fiber before or after cross-linking reactional treatment of the cellulosic fiber and respectively specifying washing shrinkage factor and a measured value of flexural rigidity determined by measurement with a Kawabata Evaluation System(KES) (R)/Metsuke [mass of a woven fabric per unit area (g/m<2> )] ratio. SOLUTION: The weight reduction processing of cellulosic fiber with a cellulolytic enzyme, etc., is carried out before or after cross-linking reactional treatment thereof by treatment with a cellulose reactional type resin. The washing shrinkage factor of the cellulosic textile structure is <=3% and the ratio B/W of a measured value B of flexural rigidity measured determined by measurement with the KES (R) to the Metsuke W is 0.0001-0.005.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fiber structure composed of cellulosic fibers, which has shape stability and a soft texture, and a method for producing the same.

[0002]

2. Description of the Related Art Conventionally, a fiber-reactive resin or a resin processing with formaldehyde vapor has been carried out for morphologically stable processing of a fiber structure composed of cellulose fibers. However, in order to obtain a high degree of morphological stability, it is necessary to add a large amount of resin, in which case the texture of the fiber structure is hardened. Various softening agents are generally used to overcome the problem, but the softening effect is limited.

As disclosed in Japanese Patent Application Laid-Open No. 7-189135, a method has been proposed in which a sewn product is subjected to form-stabilizing treatment with formaldehyde vapor and then treated with a cellulolytic enzyme. According to the method, it is difficult to uniformly treat each part of the sewn product with the enzyme, and there has been a problem that the quality of the sewn product is greatly impaired or the strength is locally greatly reduced. Another problem is that it is difficult to carry out morphologically stable processing and enzyme treatment of sewn products because it requires a special device.

[0004]

The object of the present invention is to overcome the problems of the hardening of the texture due to the above-described morphological stability processing, and to have a morphological stability of a fiber structure composed of cellulose fibers. It is to obtain a fiber structure having a soft texture and a manufacturing method thereof.

A further object of the present invention is to overcome the problems of the above-mentioned processing method for a sewn product, and to obtain a product having a high quality by a uniform enzyme treatment and having no local strength reduction.

[0006]

The fibrous structure of the present invention comprises:
In order to achieve the above purpose, it has the following configuration.

That is, in a fiber structure composed of cellulose fibers, the washing shrinkage rate is 3% or less, and KE
A fiber structure characterized in that a ratio B / W of a flexural rigidity measurement value (B) and a basis weight (W) measured by S (Kawabata Evaluation System) is 0.0001 or more and 0.005 or less.

Further, the method for producing a fiber structure of the present invention is
It has the following configuration.

That is, the method for producing a fiber structure is characterized in that the cellulose fiber is subjected to a weight reduction process before or after the step of subjecting the cellulose fiber constituting the fiber structure to a crosslinking reaction.

[0010]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in detail below.

In the present invention, the cellulose fibers include, but are not limited to, natural cellulose fibers such as cotton and hemp, and regenerated cellulose fibers such as rayon, polynosic, cupra and tencel. The fiber structure composed of cellulose fibers may be a woven fabric, a knitted fabric or a non-woven fabric substantially composed of cellulose fibers, or a sewing product thereof.

The washing shrinkage rate as used in the present invention is JIS-L1.
The value measured by the method according to 042, or the value measured by the method according to JIS-L1042 in which a similar result is obtained by changing the washing tester or the processing conditions.

The washing shrinkage of the fiber structure of the present invention must be 3% or less. If the washing shrinkage ratio exceeds 3%, the morphological stability becomes poor. This washing shrinkage rate is 2%
Is preferable and 1% or less is more preferable.

In the present invention, KES (Kawabata Evalu
ation system) is a KES bending property measuring machine (Kato), as described in Tokuo Kawabata, Textile Machinery Society of Japan (Textile Engineering), vol.26, No.10, P721-P728 (1973). TEC) is used to measure the repulsive force at each curvature when the fiber structure is bent. Then, the average value of the repulsive force between the curvatures of 0.5 and 1.5 is B (unit: g · cm ²
/ Cm), and further, this measurement is performed in each of two directions of the fiber structure, that is, the longitudinal direction and the lateral direction, and the average value is defined as B.
The ratio B / W between the value of B and the basis weight W (unit: g / m ² ) of the fiber structure is obtained.

In the fiber structure of the present invention, the ratio B / W of the flexural rigidity measurement value (B) by the KES measurement and the basis weight (W) needs to be 0.0001 or more and 0.005 or less.

B / W by this KES measurement is 0.005
If it exceeds, the texture becomes hard and the quality deteriorates. This B / W is preferably 0.004 or less, and 0.
It is more preferably 003 or less.

Next, a method for manufacturing the fiber structure of the present invention will be described.

The fiber structure of the present invention is obtained by subjecting the fiber structure to wrinkling after washing by cross-linking the cellulose constituting the cellulose fiber, that is, by subjecting it to a so-called morphological stabilizing process.

Examples of the method for cross-linking cellulose include a method of treating a fiber structure with a fibrin reaction type resin, a method of exposing the fiber structure to formaldehyde vapor, and a heat treatment in the presence of a catalyst.

Examples of the fiber-reactive resin include dimethylol ethylene urea, dimethylol urone, dimethylol triazone, dimethylol propylene urea, dimethylol hydroxyethylene urea and the like. Further, as a method for treating the fiber structure with the fibrin-reactive resin, for example, an aqueous solution of the resin is applied to the fiber structure together with a catalyst by padding, and then 80 ° C. or higher 20
A method of heat treatment at a temperature of 0 ° C. or lower can be preferably adopted. An inorganic metal salt such as magnesium chloride can be used as the catalyst.

On the other hand, formaldehyde vapor can be generated by heating an aqueous formaldehyde solution or paraformaldehyde. The heat treatment after exposing the fiber structure to this formaldehyde vapor is 60 ° C or higher 1
It is preferably performed at 60 ° C. or lower, and an acidic substance such as sulfuric acid or sulfurous acid can be used as a catalyst in that case.

Crosslinking with a fibrin reactive resin and / or formaldehyde is carried out by liquid chromatography or NM.
It can be detected using various commonly used analysis methods such as R.

In the present invention, in addition to the above-described shape-stable processing, it is necessary to carry out weight reduction processing.

The weight-reducing process in the present invention means a treatment for decomposing and removing a part of the fibers constituting the fiber structure to reduce the weight thereof. Generally known as a weight loss processing method for cellulose fibers is treatment with a cellulolytic enzyme or hydrolysis with an acid,
In the present invention, it is desirable to use the treatment with a cellulolytic enzyme.

As the cellulolytic enzyme, those obtained by culturing bacterial cells of the genus Tricoderma, the genus Fumicola, the genus Aspergills, the genus Bacillus and the like can be used. These cellulolytic enzymes are already on the market and may be used as they are.

In the present invention, the weight reduction rate of weight reduction processing is
It refers to the ratio of the portion that is decomposed and removed before and after processing, and is specifically calculated from (weight loss / weight before processing) × 100.

In the present invention, the weight reduction rate is preferably 3% or more and 10% or less from the viewpoint of imparting flexibility to the fiber structure while maintaining strength.

As a method for reducing weight, for example, an aqueous solution having the above-mentioned enzyme concentration of 1 g / l or more and 30 g / l% or less,
The fibrous structure may be immersed and treated at a temperature of 30 ° C. or higher and 90 ° C. or lower.

In the present invention, the order of the cross-linking reaction of cellulose and the weight-reducing process may be that after the cross-linking reaction, the weight-reducing process may be performed, or conversely, the weight-reducing process may be performed first. The advantage of performing the shape-stabilizing process first is that a large inter-fiber void is generated by the weight-reducing process, so that the effect of softening the texture becomes large. On the contrary, when the weight reduction process is performed first, the inter-fiber voids generated are reduced during the morphological stabilization process, so that the softening effect on the texture is reduced, but the morphological stabilization effect is increased. It may be appropriately selected according to the desired characteristics.

The shape-stabilizing process in which the fiber structure is exposed to formaldehyde vapor and heat-treated in the presence of a catalyst is generally performed on the product after being sewn. It is desirable to do this not for the product after sewing but for the cloth before sewing. The reason is that it is difficult to uniformly process each part of the sewn product in the processing of the sewn product, and there is a problem that the quality of the sewn product is greatly impaired or the strength is locally greatly reduced. In addition, it is difficult to easily perform the shape-stabilizing process and the weight-reducing process on the sewn product because a special device is required. In the present invention, such a problem can be avoided by performing the weight reduction processing in the state of the cloth before sewing.

[0031]

The present invention will now be described more specifically with reference to examples.

The evaluation of the washing shrinkage ratio and the softness of the texture in the examples was carried out by the following methods.

(1) Washing shrinkage rate The washing shrinkage rate was measured by a JI using a household washing machine.
It carried out on the following processing conditions so that the result equivalent to the washing shrinkage rate test method of S-L1042 might be obtained.

Three test pieces of about 50 cm × about 50 cm were taken, and vertical marks were made on each of the three pieces at intervals of 150 mm with a length of 300 mm. Next, put 25 liters of a liquid containing a detergent "Zab" (registered trademark of Kao Corporation) at a concentration of 0.2% into a household washing machine (Toshiba VH-1150 type),
The weight of the test piece and the additional cloth was adjusted to about 500 g, and the cloth was washed at 40 ° C. for 25 minutes. Further 40
It rinsed at 10 degreeC for 10 minutes, and dehydrated with the dehydrator. Thereafter, the test piece was taken out without squeezing, lightly dewatered by sandwiching it between dry filter papers, and then naturally dried on a horizontally placed wire net. Finally, place the test piece on a flat table, remove the artificial wrinkles and tension, measure the length between the marks on each side,
Freshly and horizontally, three average values were obtained separately. The shrinkage rate was calculated by the following formula, and was expressed as an average value of 3 sheets for each of vertical and horizontal.

Shrinkage (%) = (300−L) / 300 × 100 Here, L represents the average value (mm) of the length between the vertical marks and the horizontal marks after the treatment.

(2) Weight loss rate The weight loss rate was calculated from the absolute dry weight of the fiber structure before weight reduction processing and the absolute dry weight of the fiber structure after processing by the following formula.

Weight loss rate (%) = (absolute dry weight of fiber structure before processing-absolute dry weight of fiber structure after processing) / (absolute dry weight of fiber structure before processing) × 100 (3) B / W KES (Kawabata Evaluation System) Bending rigidity using a measuring machine, vertical mean value B (unit: g · cm ²
/ Cm) and the basis weight W (unit: g / m ² ) of the fiber structure, the ratio B / W was measured.

Example 1 Scoured and bleached cotton fabric (use of yarn: 45 count warp, 45 count weft, plain fabric, weave density: 115 warp / inch
An aqueous solution containing 6% of dimethylolhydroxyethyleneurea and 2% of magnesium chloride hexahydrate as a catalyst was applied by padding to × weft 76 lines / inch and basis weight: 110 g / m ² ). The squeezing rate was 90%. Then, the cotton fabric was dried at 100 ° C for 3 minutes and then at 160 ° C for 1 minute.
Heat treated for minutes.

Thereafter, the cotton fabric was dipped in a treatment solution containing a cellulolytic enzyme (Cellsoft L, manufactured by Novo Nordisk) at a concentration of 5 g / l and treated at 60 ° C. for 1 hour. As a result, the weight of the fabric was reduced by 5.2% as compared with the cotton fabric before the enzyme treatment.

After these two treatments, dyeing and finishing treatments were carried out by a usual method, and then the shrinkage ratio and bending rigidity of the woven fabric were measured by the above-mentioned method.
%, Width 0.8%, B is 0.270 g · cm ² / cm
And W is 104 g / m ² , and B / W is 0.0026.
Met.

On the other hand, the washing shrinkage of the cotton fabric which has not been subjected to these two treatments and which has just been subjected to the scouring and bleaching treatment is 5.5% and 5.0%, and B is 0.902 g. c
At m ² / cm, W was 110 g / m ² and B / W was 0.0082.

Example 2 Cotton fabric which has been scoured and bleached (use of yarn: warp yarn 45 count, weft yarn 45 count, plain fabric, weave density: warp 115 yarns / inch
× Weft 76 lines / inch, basis weight: 110 g / m ² ), cellulolytic enzyme (CellSoft L, manufactured by Novo Nordisk)
Is immersed in a treatment liquid containing 5 g / l of the solution at 60 ° C. for 1 hour.
Time processed. As a result, the weight of the fabric was reduced by 7.5% as compared with the cotton fabric before the enzyme treatment.

Thereafter, this cotton fabric was padded with an aqueous solution containing 6% of dimethylolhydroxyethyleneurea and 2% of magnesium chloride hexahydrate as a catalyst. The squeezing rate was 90%. This cotton fabric is 100 ℃
After being dried for 3 minutes, it was heat-treated at 160 ° C. for 1 minute.

After these two treatments, dyeing and finishing treatments were carried out by the usual methods. The washing shrinkage ratio was 0.8% and 0.7%, and B was 0.305 g.cm. ²
/ Cm, W is 102 g / m ² , and B / W is 0.0
It was 030.

Example 3 Cotton fabric which had been scoured and bleached (use of yarn: 45th warp, 45th weft, plain weave, weaving density: 115 warp / inch)
× weft 76 lines / inch, basis weight: 110 g / m ² ) was exposed to formaldehyde vapor generated from paraformaldehyde for 5 minutes in a closed reactor. The reactor temperature during the exposure was 60 ° C. Then, after the sulfurous acid gas was introduced into the reactor to expose the cloth, the temperature of the reactor was changed to 160 ° C.
And treated for 3 minutes.

Thereafter, this cotton fabric was dipped in a treatment solution containing a cellulolytic enzyme (CellSoft L, manufactured by Novo Nordisk) at a concentration of 5 g / l, and treated at 60 ° C. for 1 hour. As a result, the weight of the fabric was reduced by 6.5% as compared with the cotton fabric before the enzyme treatment.

After these two treatments, dyeing and finishing treatments are carried out by a usual method, and then the washing shrinkage ratio and the bending rigidity are measured by the above-mentioned methods.
%, Horizontal 0.9%, B is 0.237 g · cm ² / cm
And W is 103 g / m ² , and B / W is 0.0023.
Met.

Example 4 Cotton fabric that had been scoured and bleached (yarn usage: warp 45 count, weft 45 count, plain fabric, weave density: 115 warp / inch
× Weft 76 lines / inch, basis weight: 110 g / m ² ), cellulolytic enzyme (CellSoft L, manufactured by Novo Nordisk)
Is immersed in a treatment liquid containing 5 g / l of the solution at 60 ° C. for 1 hour.
Time processed. As a result, the weight of the fabric was reduced by 7.3% as compared with the cotton fabric before the enzyme treatment.

The cotton fabric was then introduced into a closed reactor and exposed to formaldehyde vapor generated from paraformaldehyde for 5 minutes. The reactor temperature during the exposure was 60 ° C. Next, after sulfurous acid gas was flown into the reactor to expose the cloth, the temperature of the reactor was raised to 160 ° C. and treated for 3 minutes.

After these two treatments, dyeing and finishing treatments were carried out by a usual method, and then the washing shrinkage ratio and the bending rigidity were measured by the above-mentioned methods.
%, Width 0.8%, B is 0.286 g · cm ² / cm
And W is 102 g / m ² , and B / W is 0.0028.
Met.

Comparative Example 1 Scoured and bleached cotton fabric (use of yarn: 45 count warp, 45 count weft, plain fabric, weave density: 115 warp / inch
An aqueous solution containing 6% of dimethylolhydroxyethyleneurea and 2% of magnesium chloride hexahydrate as a catalyst was applied by padding to × weft 76 lines / inch and basis weight: 110 g / m ² ). The squeezing rate was 90%. Then, the cotton fabric was dried at 100 ° C for 3 minutes and then at 160 ° C for 1 minute.
Heat treated for minutes.

After that, when the washing shrinkage ratio and the flexural rigidity are measured, the washing shrinkage ratio is 0.9% vertically, 0.9% horizontally, and B
Is 0.957 g · cm ² / cm and W is 110 g / m ²
And B / W was 0.0087. In this case, morphological stability was obtained but flexibility was poor.

Comparative Example 2 Scoured and bleached cotton fabric (yarn use: warp 45 count, weft 45 count, plain fabric, weave density: 115 warp / inch
× weft 76 lines / inch, basis weight: 110 g / m ² ) was exposed to formaldehyde vapor generated from paraformaldehyde for 5 minutes in a closed reactor. The reactor temperature during the exposure was 60 ° C. Then, after the sulfurous acid gas was introduced into the reactor to expose the cloth, the temperature of the reactor was changed to 160 ° C.
And treated for 3 minutes.

After that, when the washing shrinkage ratio and the bending rigidity were measured, the washing shrinkage ratio was 1.0% vertically and 1.0% horizontally, and
Is 0.913 g · cm ² / cm and W is 110 g / m ²
And B / W was 0.0083. In this case, morphological stability was obtained but flexibility was poor.

Comparative Example 3 Cotton fabric that has been scoured and bleached (yarn usage: warp 45 count, weft 45 count, plain fabric, weave density: 115 warp / inch
× Weft 76 lines / inch, basis weight: 110 g / m ² ), cellulolytic enzyme (CellSoft L, manufactured by Novo Nordisk)
Is immersed in a treatment liquid containing 5 g / l of the solution at 60 ° C. for 1 hour.
Time processed. As a result, the weight of the fabric was reduced by 7.5% as compared with the cotton fabric before the enzyme treatment.

After that, when the washing shrinkage ratio and the bending rigidity are measured, the washing shrinkage ratio is 5.5% vertically and 5.3% horizontally, and B
Is 0.275 g · cm ² / cm, W is 102 g / m ²
And B / W was 0.0027. In this case, flexibility was obtained but morphological stability was poor.

Examples 5 to 8 Example 1 except that the kind of the fibrin reactive resin was changed.
The same was done. Table 1 shows the results. All had excellent morphological stability and flexibility.

[0058]

[Table 1] Examples 9 to 12 The same procedure as in Example 1 was carried out except that the drying temperature and the heat treatment temperature were changed. Table 2 shows the results. All had excellent morphological stability and flexibility.

[0059]

[Table 2] Examples 13 to 15 The same procedure as in Example 3 was performed except that the temperature of the formaldehyde vapor and the heat treatment temperature were changed. Table 3 shows the results.
All had high morphological stability and flexibility.

[0060]

[Table 3]

[0061]

Industrial Applicability According to the present invention, it is possible to provide a fiber structure having a high degree of morphological stability and excellent in flexibility and made of a cellulose fiber which is most suitable for a shirt cloth, particularly a dress shirt and casual use.

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[Procedure amendment]

[Submission date] February 29, 1996

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] 0020

[Correction method] Change

[Correction contents]

[0020] As here cellulose reactive resin include dimethylol ethylene urea, dimethylol uronic, dimethylol triazone, dimethylol propylene urea and dimethylol di hydroxyethylene urea. Further, as a method for treating the fiber structure with the fibrin-reactive resin, for example, an aqueous solution of the resin is applied to the fiber structure together with a catalyst by padding, and then 80 ° C. or higher 20
A method of heat treatment at a temperature of 0 ° C. or lower can be preferably adopted. An inorganic metal salt such as magnesium chloride can be used as the catalyst.

[Procedure amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0038

[Correction method] Change

[Correction contents]

Example 1 Scoured and bleached cotton fabric (use of yarn: 45 count warp, 45 count weft, plain fabric, weave density: 115 warp / inch
× weft 76 present / inch, basis weight: 110g / in m ^2), 6% of dimethylol di hydroxyethylene urea, was applied by padding an aqueous solution containing 2% of magnesium chloride hexahydrate as catalyst. The squeezing rate was 90%. Then, the cotton fabric was dried at 100 ° C. for 3 minutes and then heat-treated at 160 ° C. for 1 minute.

[Procedure 3]

[Document name to be amended] Statement

[Correction target item name] 0043

[Correction method] Change

[Correction contents]

[0043] Thereafter, the cotton fabric in dimethylol di hydrate <br/> Rokishiechiren urea 6% was applied by padding an aqueous solution containing 2% of magnesium chloride hexahydrate as catalyst. The squeezing rate was 90%. This cotton fabric is 100 ℃
After being dried for 3 minutes, it was heat-treated at 160 ° C. for 1 minute.

[Procedure amendment 4]

[Document name to be amended] Statement

[Correction target item name] 0051

[Correction method] Change

[Correction contents]

Comparative Example 1 Scoured and bleached cotton fabric (use of yarn: 45 count warp, 45 count weft, plain fabric, weave density: 115 warp / inch
× weft 76 present / inch, basis weight: 110g / in m ^2), 6% of dimethylol di hydroxyethylene urea, was applied by padding an aqueous solution containing 2% of magnesium chloride hexahydrate as catalyst. The squeezing rate was 90%. Then, the cotton fabric was dried at 100 ° C. for 3 minutes and then heat-treated at 160 ° C. for 1 minute.

Claims (15)

[Claims] 1. A fiber structure made of cellulose fibers, having a washing shrinkage of 3% or less and KES (Kawaba).
The ratio B / W of the flexural rigidity measurement value (B) and the basis weight (W) measured by the ta evaluation system is 0.0001 or more.
A fiber structure characterized by being 005 or less. 2. The fiber structure according to claim 1, wherein the cellulose fibers are crosslinked with a fibrin-reactive resin and / or formaldehyde. 3. The fiber structure according to claim 1, which has a washing shrinkage ratio of 2% or less. 4. The fiber structure according to claim 1, which has a washing shrinkage ratio of 1% or less. 5. The fiber structure according to claim 1, wherein B / W is 0.0001 or more and 0.004 or less. 6. The fiber structure according to claim 1, wherein B / W is 0.0001 or more and 0.003 or less. 7. A method for producing a fiber structure, which comprises reducing the weight of the cellulose fiber before or after the step of subjecting the cellulose fiber constituting the fiber structure to a crosslinking reaction. 8. The method for producing a fiber structure according to claim 7, wherein the cellulose is impregnated with a fibrin reaction type resin and then crosslinked by heat treatment. 9. The method for producing a fiber structure according to claim 8, wherein the temperature of the heat treatment is 80 ° C. or higher and 200 ° C. or lower. 10. The method for producing a fiber structure according to claim 7, wherein the cellulose fiber is exposed to formaldehyde vapor and subjected to heat treatment in the presence of a catalyst to crosslink. 11. The temperature of the heat treatment is 60 ° C. or higher and 160 ° C.
The method for producing a fiber structure according to claim 10, wherein: 12. The method for producing a fiber structure according to claim 7, wherein the weight-reducing process is a weight-reducing process of cellulose fibers with a cellulolytic enzyme. 13. The method for producing a fiber structure according to claim 12, wherein the weight loss rate is 3% or more and 10% or less. 14. A fibrous structure is immersed in an aqueous solution having a cellulolytic enzyme concentration of 1 g / l or more and 30 g / l or less for 30 minutes.
The method for producing a fiber structure according to claim 12, wherein the treatment is performed at a temperature of not less than 90 ° C and not more than 90 ° C. 15. The method for manufacturing a fiber structure according to claim 7, wherein, when sewing the fiber structure, the weight reduction process is performed before the sewing.