JPH0615742B2 - Silk fiber salt shrink processing method - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a silk fiber salt shrinking method, and more specifically, a silk fiber salt shrinking method for obtaining a uniform and reproducible grained fabric or stretch fabric. It is about.

[Prior art] Salt shrinking is well known as one of the ancient chemical processes for silk fibers, and Ca (NO ₃ ) ₂ , CaCl ₂ , ZnCl _{2 and the} like are typical neutral salts of salt shrinking. Are listed as. Using these concentrated solutions of neutral salt, the silk fibers are treated at high temperature for a short time,
Gravel and stretch fabrics are made by significantly swelling and shrinking.

[Problems to be solved by the invention]

However, salt shrink processing is based on the concentration (specific gravity) of the neutral salt solution.
Even if the temperature or temperature fluctuates even a little, it quickly grows into shrinkage plaques, and the size of the grain and the stretchability tend to differ. In addition, there may be a case of partial dissolution deterioration. This is true both within and between lots, and it is difficult to obtain fibers with uniform warpage and stretchability with good reproducibility, and even if manual production is performed, general industrial production is still practiced. Not a big cause.

[Means for solving problems]

The inventors of the present invention treat the silk fiber with a water-soluble epoxy compound prior to the salt-shrinking process, so that during the salt-shrinking process, shrinkage unevenness occurs even if the concentration or temperature of the neutral salt aqueous solution slightly changes. The present invention has been completed by finding that a woven fabric having uniform warp and stretchability can be obtained with good reproducibility.

That is, the present invention is a method for shrinking a silk fiber, which comprises treating the silk fiber with an aqueous solution containing a water-soluble epoxy chemical and a catalyst, and then treating it with a concentrated solution of a neutral salt.

The present invention will be described in detail below.

Examples of the water-soluble epoxy compound used in the present invention include ethylene glycol, polyethylene glycol, propylene glycol, polypropylene glycol, glycerin, sorbitol, polyglycerol, pentaerythritol, tris (2hydroxyethyl) isocyanurate, trimethylolpropane, neopentyl glycol. , Phenol ethylene oxide, lauryl alcohol ethylene oxide mono, and polyglycidyl ethers. Polyglycidyl ethers of ethylene oxide and propylene oxide such as polyglycerol, ethylene glycol, polyethylene glycol, propylene glycol, polypropylene glycol, phenol ethylene oxide and lauryl alcohol ethylene oxide are preferred. In particular, ethylene glycol, polyethylene glycol, propylene glycol,
Diglycidyl ether of polypropylene glycol is preferable in terms of its effect. These water-soluble epoxy compounds are used by dissolving them in water, but when the solubility is low, they are dissolved in a medium containing a small amount of an organic solvent such as dioxane or isopropyl alcohol and water. The amount of the water-soluble epoxy compound applied varies depending on the epoxy equivalent and the like, but is 1 to 20% by weight, preferably 3 by weight in the dipping method, relative to the silk fiber.
10 to 10% by weight, 3 to 50% by weight in the pad-steam method and the pad-dry-steam method, preferably 6 to 40%
% By weight, 5 to 50% by weight in the cold batch method, and preferably 10 to 40% by weight.

The catalyst used in the present invention is a neutral salt, a weak alkaline salt, an alkaline salt, an acidic salt, an alkali metal hydroxide, aqueous ammonia, and amines. The neutral salts are preferably sodium and potassium salts of sulfuric acid, hydrochloric acid, nitric acid, thiocyanic acid and thiosulfuric acid, and the weakly alkaline salts are tartaric acid, citric acid, acetic acid, propionic acid and hydrogencarbonic acid sodium salts, potassium salts and potassium salts. The alkaline salt is preferably carbonic acid, sodium salt of silicic acid and aminopolycarboxylic acid, magnesium chloride is preferred as the acidic salt, and amines are ethylenediamine, diethylenetriamine, triethylenetetramine, dimethylaminopropylamine, m- Phenylenediamine, 2,4,6-tris (dimethylaminomethyl) phenol, 2-methylimidazole and dimethylaniline are preferred. The catalyst preferably has a pH of the processing liquid of 9 or higher. The amount of the catalyst used is 0.3 to 15% by weight, preferably 1 to 15% by weight, based on the silk fiber.
Is.

As a method for treating silk fiber with a water-soluble epoxy compound and a catalyst, an immersion heating method, a pad-steam method, a pad-dry-steam method, a cold batch method or the like can be used. In the immersion heating method, the treatment is carried out at a temperature of, for example, 50 to 110 ° C, preferably 60 to 95 ° C. In the pad-steam method, for example, 50 to 200% by weight, preferably 80 to 120% by weight, of an aqueous liquid is applied to silk fibers, and then steaming is performed with saturated steam at 120 ° C. or less, preferably 110 ° C. or less. In the pad-dry-steam method, for example, 50 to 200% by weight, preferably 80 to 120% by weight, of an aqueous liquid is applied to silk fibers, and then 50 to 1%.
Dry at a temperature of 00 ° C. and then steam with heated steam below 150 ° C. or steam with saturated steam below 120 ° C., preferably below 110 ° C. In the cold batch method, for example, an aqueous liquid of 50 to 200% by weight, preferably 80 to 120% by weight is applied to silk fibers, and then, without being dried, for example, it is rolled up and covered with a film or the like to evaporate water. Place at room temperature with protection. Room temperature is 1
The temperature is 0 ° C or higher, preferably 20 ° C or higher and 40 ° C or lower, and the time is 20 hours or longer, preferably 20 hours or longer and 50 hours or shorter.

After the treatment, it is washed with hot water and soaped according to the usual method.

What is important in the present invention is that the silk fiber treated with an aqueous solution containing a water-soluble epoxy compound and a catalyst has a solubility of 10 to 40% by weight when immersed in a 5% by weight aqueous sodium hydroxide solution at 65 ° C. for 60 minutes. , Preferably 12-
That is, it is set to 35% by weight. If it is less than 10% by weight, the effect of salt shrinking will be lost, and if it is more than 40% by weight, the stabilizing effect of salt shrinking will be poor. The degree of stabilization should also take into account the strength of the salt shrinking process. When performing the strong salt shrinking process, the alkali solubility is set to be low, and when performing the weak salt shrinking process, the alkali solubility is set to be high.

As the neutral salt used in the present invention, in silkworm silk,
_{Ca (NO 3) 2, CaCl} 2 or the like, in the wild silkworms silk ZnCl _2, Ca (CN
S) _{2 and the} like. Ca (NO ₃ ) ₂ is particularly preferable in terms of the stabilizing effect. An immersion heating method can be used as a method of treating the silk fibers with a neutral salt. The treatment concentration at this time varies depending on the target shrinkage ratio, but in the case of Ca (NO ₃ ) ₂ , it is 40
-60% by weight, preferably 45-55% by weight. The treatment temperature is 70 to 100 ° C., preferably 80 to 90.
C., and the treatment time is 0.5 to 20 minutes, preferably 1 to 1
0 minutes.

[Action]

Salt shrinkage is a process that causes shrinkage by breaking the hydrogen bond between tyrosine and an adjacent fibroin molecule. However, if the OH group of tyrosine is blocked with an epoxy compound prior to salt shrinkage, shrinkage can be controlled depending on the degree of silk shrinkage. The susceptibility of the fiber to changes in the concentration and temperature of the neutral salt solution can be mitigated.

〔Example〕

 Hereinafter, the present invention will be described in detail based on examples.

Examples 1 to 4 and Comparative Examples 1 and 2 Fuji silk having a warp density of 122 yarns / inch and a weft yarn density of 105 yarns / inch using 140-count twin yarns as warp yarns was refined by an ordinary method, and ethylene glycol was used as an epoxy compound. Diglycidyl ether (manufactured by Nagase Kasei Kogyo, Denacol EX-810: trademark) 5 to 30 g /, and an aqueous solution containing 100 g / 1 of sodium citrate as a catalyst in a bath ratio of 1:
After dipping at 50 and treatment at 90 ° C. for 1 hour, hot water washing, soaping, hot water washing, water washing and drying were performed.

Solubility of the obtained processed products and unprocessed products (5% NaOH, 65%
The solubility% by weight at 60 ° C. for 60 minutes) is shown in Table 1.

The epoxy compound-treated cloths having different alkali solubilities shown in Table 1 were dipped in an aqueous solution containing 48% by weight of Ca (NO ₃ ) ₂ ,
After treatment at 90 ° C. for 1 minute, washing with hot water, washing with water and drying were performed. Table 2 shows the shrinkage rate and processing uniformity. The shrinkage rate is shown by the average value of 5 points, and the uniformity of processing is shown by the difference between the maximum value and the minimum value of the shrinkage rate in the warp direction.

As is clear from Table 2, the products obtained in the examples of the present invention have a high shrinkage ratio and there is no variation in the shrinkage ratio.

〔The invention's effect〕

As described above, according to the silk fiber salt shrinking method of the present invention, it is possible to reproducibly obtain a woven fabric having uniform warp and stretchability. The effect of the present invention is remarkable in view of the fact that it is difficult to obtain a product having uniform warp and stretchability with good reproducibility in the conventional technique.

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Claims (2)

[Claims] 1. A process for shrinking a silk fiber, which comprises treating the silk fiber with an aqueous liquid containing a water-soluble epoxy compound and a catalyst, and then with a concentrated solution of a neutral salt. 2. A silk fiber treated with an aqueous solution containing a water-soluble epoxy compound and a catalyst is set to have a solubility of 10 to 40% by weight when immersed in a 5% by weight aqueous sodium hydroxide solution at 65 ° C. for 60 minutes. The salt shrinking method for silk fiber according to claim 1, wherein