JP3107755B2 - Dyeing method for protein fiber products and dye fastness stabilizer used therefor - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for dyeing protein fiber products made from wool, silk, etc. with an acid mordant dye, and to a dye fastness stabilizer for potting used in the method.

[0002]

2. Description of the Related Art In this type of dyeing method, an acid mordant dye, which is generally called a commercially available purified chromium dye, is widely used as a dye having a high color fastness. On the other hand, when dyeing is performed using an incompletely purified acid mordant dye, the fastness to contamination, particularly the fastness to dyeing for potting, is considerably reduced due to the presence of many impurities. In order to prevent this, conventionally, the dyeing method was performed in two baths, and after dyeing the protein fiber product with the acid mordant dye in the first bath, the protein fiber product was placed in another dyeing bath, and ammonia was added at 60 ° C for 20 minutes in the second bath. Processing is in progress.

[0003]

However, in the above two-bath dyeing method, after dyeing with an acid mordant dye, the protein fiber product must be taken out of the dye bath and placed in another dye bath. Second, there was a problem that the irritating odor of ammonia leaked to the outside of the dyeing bath in the second bath, which extremely deteriorated the working environment. For this reason, this dyeing method was considerably avoided at the actual dyeing site.

[0004] An object of the present invention is to provide a simple bath without changing the dyeing bath and to emit a strong irritating odor from the dyeing bath without changing the dyeing bath even when dyeing with an incompletely purified acid mordant dye.
It is an object of the present invention to provide a method for dyeing a protein fiber product, which dyes a protein fiber product with high dyeing fastness against potting, and a dyeing fastness stabilizer used in the method.

[0005]

The invention according to claim 1 is
The protein fiber product put in the dyeing bath is 90-1 by acid mordant dye.
After dyeing at 00 ° C., the temperature was lowered to 60 ° C.
Solid at room temperature and atmospheric pressure with a pKa of 6.0 to 14.0.
2.5-40% o of a water-soluble ammonium salt of a weak acid
This is a method for dyeing a protein fiber product in which wf is added and treated at 60 ° C. Here, “pKa” is an acid dissociation exponent, which means (−log Ka) when the ionization constant of a weak acid is Ka, that is, the logarithmic value of the reciprocal of the acid dissociation constant. A protein fiber product is dyed with an insufficiently refined acidic mordant dye, and the dye is fixed to the protein fiber product by adding dichromate to form a color, and then treated with the above-mentioned predetermined amount of a water-soluble ammonium salt. Adhered impurities and unreacted chromium dye residues are removed. As a result, an object to be dyed having high fastness to potting can be obtained, and since it is an ammonium salt, it is possible to greatly reduce an irritating odor such as ammonia during the dyeing operation.

The invention according to claim 2 is the invention according to claim 1, which is a method for dyeing a protein fiber product, wherein the acidic mordant dye is CIBlack11. Color Index is CI Black 11
Acid mordant dyes are particularly poorly purified and have extremely poor dye fastness to potting, so when CI Black 11 dye is used as the acid mordant dye,
This dyeing method is preferred.

The invention according to claim 3 is used in the dyeing method according to claim 1, and is solid at room temperature and atmospheric pressure and has a pKa of 6.
It is a dye fastness stabilizer comprising a water-soluble ammonium salt of a weak acid of 0 to 14.0. Unlike conventional dye fastness stabilizers having a strong irritating odor such as ammonia, the ammonium salt does not emit a stimulating odor so much that the working environment can be improved.

[0008]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in detail. The protein fiber product to be dyed according to the present invention includes wool, cashmere hair, animal hair fibers such as alpaca hair, silkworms, cocoon fibers obtained from cocoons such as wild silkworms, or wool, silk threads made from these fibers, or , Knitted and non-woven fabrics made from the fibers or yarns of

The ammonium salt of the present invention is solid at room temperature and atmospheric pressure and has an acid dissociation index pKa of 6.0 to 1
The compound is an ammonium salt of a weak acid of 4.0 and is soluble in water. Examples of this ammonium salt include ammonium carbonate (an ammonium salt of a weak acid (pKa = 6.35)) and ammonium bicarbonate (a weak acid (pKa = 1).
0.33), ammonium sulfide (ammonium salt of weak acid (pKa = 7.02)), etc.
Catechol (pKa = 9.23) ammonium salt. Ammonium hydrogen carbonate is preferred from a practical point of view. In order to remove impurities and chromium unreacted dye residue adhering to the material to be dyed, pKa is 6.0 to 14.0.
It is necessary to be an ammonium salt formed by reacting with a weak acid. Preferably, the pKa is 6.0 to 11.
0. Also, since it is an ammonium salt, it does not have a pungent odor like ammonia.

The amount of the ammonium salt used is 2.5 to 40% by weight (hereinafter referred to as "% ow") based on the weight of the protein fiber product.
f ”(on the weight of fiber). Preferably it is 5 to 20% owf. If it is less than 2.5% owf, the amount of ammonium ions generated is too small to produce an effect, and if it exceeds 40% owf, it is effective, but it is not economical and adversely affects physical properties such as texture of protein fiber. Is used in the above range. An effective treatment temperature of ammonium salt is 60 ° C. If the temperature exceeds 60 ° C., the decomposition of the ammonium salt will be accelerated and a sufficient effect cannot be expected.
If the temperature is lower than 60 ° C., the amount of ammonium salt used increases, and the above-mentioned adverse effects are caused.

[0011]

EXAMPLES Examples of the present invention will be shown below, but the technical scope of the present invention is not limited to the following examples.

Example 1 The following protein fiber product was dyed in one bath based on the time chart shown in FIG. That is,
The warp is 2/22 meter count x 18 / cm and the weft is 2
A plain weave cloth of / 22 meter count x 18 / cm was prepared. This wool cloth was put into a mini-color dyeing tester (manufactured by Texam Giken Co., Ltd.) at a bath ratio of 1:20. Next, 6.0% owf of CI Black 11 (Sunchromine BLACK ET conc .; manufactured by Sumitomo Chemical Co., Ltd.) was collected, and this acidic mordant dye was put into a dye bath together with anhydrous sodium sulfate, a leveling agent, and acetic acid.
The temperature was raised from 97 ° C. to 97 ° C. at a rate of 1.0 ° C./min, and dyed for 40 minutes. After a lapse of 40 minutes, formic acid was added to the dyeing liquor and dyed for 5 minutes to sufficiently exhaust the dye. Subsequently, sodium dichromate was added to the dyeing liquor and treated for 30 minutes to fix and develop the dye. After the temperature of the dyeing liquor was lowered to 60 ° C., ammonium bicarbonate (manufactured by Ube Industries, Ltd.) 10% o was used as an ammonium salt.
wf was added to the liquor and treated for 20 minutes. After 20 minutes,
After further cooling with water, the dyeing was completed. The wool cloth was taken out of the dyeing tester, washed with water and dried to obtain a dyed cloth.

Example 2 The same Panama wool cloth as in Example 1 was prepared, dyed in one bath based on the time chart shown in FIG. 1, and cooled to 60 ° C. 4. ammonium sulfide as an ammonium salt;
After adding 0% owf and treating for 20 minutes, it was further cooled to complete the staining. The wool cloth was taken out of the dyeing tester, washed with water and dried to obtain a dyed cloth.

<Comparative Example 1> The same Panama wool cloth as in Example 1 was prepared, dyed in one bath based on the time chart shown in FIG. 1, and cooled to 60 ° C. After adding 5.0% owf of ammonium acetate (ammonium salt of weak acid (pKa = 4.56)) and treating for 20 minutes, it was further cooled to complete the staining. The wool cloth was taken out of the dyeing tester, washed with water and dried to obtain a dyed cloth.

Comparative Example 2 A dyeing method for a protein fiber product was performed in two baths. That is, the same Panama wool cloth as in Example 1 was prepared, dyed in the same manner as in Example 1 until treated with sodium dichromate for 30 minutes, then cooled to 40 ° C., washed with water, and dried to obtain a dyed cloth. Was. Next, 3.0% owf of aqueous ammonia (28%) was put into a beaker, and the aqueous ammonia solution was heated to 60 ° C. at a bath ratio of 1:20.
The dyed cloth taken out from the dyeing tester was put into this beaker and treated for 20 minutes.

<Comparison Test and Evaluation> The dyed fabrics of Examples 1 and 2 and Comparative Examples 1 and 2 were examined for dye fastness in accordance with JIS L 0875 “Testing method for dyeing fastness against potting”. Table 1 shows the results.

[0017]

[Table 1]

As is evident from Table 1, pK in one bath dyeing
The dyed fabric of Comparative Example 1 using ammonium acetate, which is an ammonium salt of a weak acid having a of less than 6, had a good fastness to discoloration and fading, but a low level of stain fastness of class 2. On the other hand, the dyed fabrics of Examples 1 and 2 using ammonium bicarbonate and ammonium sulfide, which are ammonium salts of weak acids having a pKa in the range of 6 to 14 in one-bath dyeing, show the discoloration fastness and discoloration fastness. The contamination fastness was also good. The dyed fabric of Comparative Example 2 using ammonia in the second bath in the two-bath dyeing had good fastness to discoloration and fastness and good stain fastness. Was painful. On the other hand, during the dyeing of Example 1, Example 2, and Comparative Example 1, the odor was slightly drifted.

[0019]

As described above, by removing impurities and the like adhering to a material to be dyed by using the ammonium salt of the present invention, the irritating odor of ammonia in one bath and during the operation is greatly reduced. Thus, a protein fiber product having high robustness against potting contamination can be obtained.

[Brief description of the drawings]

FIG. 1 is a time chart showing the dyeing method of Example 1, Example 2, and Comparative Example 1.

Continuation of the front page (58) Field surveyed (Int.Cl. ⁷ , DB name) D06P 3/16 D06P 1/39 D06P 1/673 D06P 5/22

Claims (3)

(57) [Claims] 1. A protein fiber product placed in a dye bath is dyed at 90 to 100 ° C. with an acid mordant dye, and then cooled to 60 ° C. The dye bath is solid at room temperature and atmospheric pressure and has a pKa of 6 A method for dyeing a protein fiber product, wherein a water-soluble ammonium salt of a weak acid having a pH of from 0.0 to 14.0 is added at 2.5 to 40% owf and treated at 60 ° C. 2. The method according to claim 1, wherein the acidic mordant dye is CI Black 11. 3. A dye fastness stabilizer comprising a water-soluble ammonium salt of a weak acid which is solid at room temperature and atmospheric pressure and has a pKa of 6.0 to 14.0, which is used in the dyeing method of claim 1.