KR100513565B1 - Dyeing Process of fibers using reactive anionic agent and Amur cork tree extract - Google Patents

Abstract

The present invention is an anion that can ionically bond with a yellow wall extraction pigment having a reactive group and a cation (+) to form a covalent bond with the fiber to a fiber having no special anion (-) group such as cotton, ramie, burlap, rayon, and the like. After pre-treatment of the reactive anionizing agent having a (-) group to form a covalent bond between the fiber and the reactive anionizing agent, the fiber having a plurality of anion (-) groups is formed by dyeing the covalent bond-formed fiber with a yellow wall extraction pigment. By combining with the yellow wall extraction dye having a cationic (+) group by the electrostatic attraction, not only can the dyeing amount of berberine be greatly improved, but also the dye is not removed even when washed with water. In the dyeing method, Sodium4- (4,6-dichloro- [1,3, which is 87.5 to 93.3% by weight of water, 5 to 10.0% by weight of sodium sulfate, 0.5 to 1.5% by weight of sodium carbonate, and a reactive anionic agent 5] dissolving 0.2 to 1.0 wt% of triazin-2-ylamino) -benzenesulfonate (S1); Immersing a predetermined amount of fibers in a dissolved aqueous solution at a temperature in the range of 30 to 40 ° C. for 1 to 2 hours such that a covalent bond is formed between the fibers and the reactive anionizing agent (S2); Washing the fiber in which the covalent bond is formed several times with water (S3); Dissolving 0.1 to 1.0% by weight of sodium carbonate in 94.0 to 99.8% by weight of water, and then dissolving 0.1 to 5.0% by weight of yellow wall extraction pigment to prepare a dye (S4); Dyeing the above-described reactive anionizing agent treated and washed fibers with a prepared dye at a temperature in the range of 35 to 45 ° C. for 30 to 50 minutes (S5); Washing the dyed fibers (S6); And a method of dyeing the fibers using the reactive anionizing agent and the yellow wall extraction pigment, characterized in that the step of drying the washed fibers (S7).

Description

Dyeing process of fibers using reactive anionic agent and Amur cork tree extract}

The present invention relates to a method for dyeing fibers using a reactive anionizing agent and a yellow wall extracting dye, and more particularly, to a fiber having no special anion (-) group, such as cotton, ramie, burlap, and rayon, with a covalent bond with the fiber. After pre-treatment of the reactive anionizing agent having both a reactive reactive group and a yellow wall extraction pigment having a cation (+) and an anionic (-) group capable of ion bonding to form a covalent bond between the fiber and the reactive anionic agent, By dyeing the formed fiber with the yellow wall extraction dye, the fiber has a large number of anion (-) groups, and the yellow wall extraction dye having a cation (+) group is bonded to each other by electrostatic attraction, thereby greatly improving the dyeing amount of berberine. In addition, the dye is not removed even when washed.

In general, the yellow wall extract is extracted from the yellow wall, one of the natural dyeing materials for dyeing cotton fabrics, ramie, burlap, silk, wool, and other fibers, and the yellow wall extract is a light yellow berberine, which is a main dye component. Contains a large amount of natural dyes.

However, berberine has a nitrogen atom (N) having a cation (+) in its molecular structure, as can be seen in the following chemical structure, and carboxylic acid (-COOH ↔-COO) in the molecular structure such as silk, wool and nylon ^­ + H ⁺ ) such as anion (-) group is good dyeing through ionic bonds due to electrostatic attraction, but almost dyed to cellulose fibers such as cotton, hemp, burlap, rayon, etc. that do not have a special anion (-) group This does not have the problem.

[Chemical Structure]

Chemical structure of berberine

Conventionally, in order to overcome this problem, cellulose fibers such as cotton fabrics were embedded with tannic acid before dyeing, and then cellulose fibers embedded with tannic acid were dyed with berberine, a yellow wall extract pigment.

However, the yellow wall extraction pigment berberine was more stained when tannin acid was embedded and dyed with berberine, a yellow wall extraction pigment, but the tannin acid dye was not as large. Since it is slightly dark yellow itself, dyeing it with berberine such as tannin acid-embedded cotton fabric does not show the light yellow inherent in berberine, but dyes the dark orange color, and tannic acid, which is highly soluble in water, adheres to fibers. Not only because it is adsorbed, it is continuously removed during washing, as well as tannic acid itself, as well as the berberine dye is also removed, there was a problem that the wash fastness (durability for washing) is very low.

Accordingly, an object of the present invention, in order to solve the problems of the conventional dyeing method of the staining of the yellow-walled extraction pigment is not good, to the fibers that do not have a special anion (-) group, such as cotton, ramie, burlap, rayon, The covalent bond between the fiber and the reactive anionic agent was formed by pretreatment of the reactive anionic agent having both a reactive group capable of forming a covalent group and a yellow wall extraction pigment having a cation (+) and an anionic (-) group capable of ion bonding. Afterwards, the covalently bonded fibers are dyed with yellow wall extraction pigments, and the fibers have a large number of anion (-) groups, and the yellow wall extraction pigments having cationic (+) groups are bonded to each other by electrostatic attraction to greatly increase the amount of berberine dyeing. Not only can it be improved, but the dyeing room of the fiber using reactive anionizing agent and yellow wall extracting dye to prevent dye removal even when washed It is to provide a.

In order to achieve the above object, the dyeing method of the fiber using the reactive anionizing agent and the yellow wall extracting dye according to the present invention is 87.5 to 94.3% by weight of sodium sulfate, 5 to 10.0% by weight of sodium carbonate, 0.5 to 1.5% by weight of sodium carbonate, and reactive type. Dissolving 0.2% to 1.0% by weight of anionic agent (S1); Immersing a predetermined amount of fibers in a dissolved aqueous solution at a temperature in the range of 30 to 40 ° C. for 1 to 2 hours to form a covalent bond between the fibers and the reactive anionizing agent (S2); Washing the fiber in which the covalent bond is formed several times with water (S3); Dissolving 0.1 to 1.0% by weight of sodium carbonate in 94.0 to 99.8% by weight of water, and then dissolving 0.1 to 5.0% by weight of yellow wall extracting dye to prepare a dye (S4); Dyeing the treated anionized and treated fibers with a prepared dye at a temperature in the range of 35 to 45 ° C. for 30 to 50 minutes (S5); Washing the dyed fibers (S6); And drying the washed fibers (S7).

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings such that those skilled in the art can easily implement the present invention.

1 is a flow chart showing the dyeing method of the fiber using the reactive anionizing agent and the yellow wall extracting dye according to the present invention, dissolution of the reactive anionizing agent (S1), covalent bond formation between the fiber and the reactive anionizing agent (S2), It consists of washing (S3), dye preparation (S4), dyeing (S5), washing with water (S6) and drying step (S7).

First, sodium sulfate, sodium carbonate and the reactive anionic agent are dissolved in water (S1).

If the blending ratio of sodium sulfate is less than 5.0% by weight, the reactive anionizing agent does not adhere to the fiber as much as possible, and if it exceeds 10.0% by weight, the reactive anionic or sodium sulfate is not dissolved. If sodium carbonate is less than 0.5% by weight, the reactive anionic The reaction to the fiber did not occur sufficiently, and if it exceeds 1.5% by weight, it became excessive and not economical, and the fixed anionizing agent was hydrolyzed again to separate from the fiber. In addition, since the reactive anionizing agent is for imparting anionicity to the fiber, if less than 0.2% by weight, sufficient amount of anion groups cannot be imparted to the fiber. Since the anionizing agent no longer reacts with the fiber even when it is used in excess of%, there is a problem in that the anionizing agent is lost and the economy is not good. Thus, 87.5 to 94.3% by weight of water is 5 to 10.0% by weight of sodium sulfate, 0.5 to 1.5% by weight of sodium carbonate and It is preferable to dissolve 0.2 to 1.0% by weight of the reactive anionic agent.

At this time, the reactive anionic agent Sodium 4- (4,6-dichloro- [1,3,5] triazin-2-ylamino) -benzenesulfonate} represented by Cyanuric chloride represented by It is synthesized by reacting with sulfanilic acid represented by.

Thereafter, a certain amount of fibers are immersed in an aqueous solution in which the reactive anionic agent is dissolved, so that a covalent bond is formed between the fiber and the reactive anionic agent (S2), so that the fibers have many anionic groups. At this time, the reactive anionizing agent is a low temperature reaction type, and can be easily combined with cellulose fibers even at room temperature, so it is not necessary to apply additional heat, but considering the dissolution of additives such as sodium sulfate and the reaction type anionizing agent or uniformity of treatment. It is preferable to process for 1-2 hours at the temperature of 30-40 degreeC.

In this case, considering the efficiency of the treatment, it is preferable to set the ratio of the fiber and the treatment liquid (weight of the fiber: the weight of the treatment liquid) to 1:20, but it is not necessarily limited thereto.

If the treatment temperature of the anionizing agent is less than 30 ℃ not only may not sufficiently dissolve the additives and the reactive anionic agent, but also the processing time is long, and if it exceeds 40 ℃ to be heated by a separate heating means good economical There is a problem in that the fixation rate of the anionizing agent to the fiber is reduced.

If the treatment time is less than 1 hour, sufficient covalent bonds cannot be formed between the anionizing agent and the fiber. If the treatment time is more than 2 hours, the productivity is lowered, so the treatment is preferably performed for 1 to 2 hours.

The covalent bond formed with the reactive anionizing agent is washed with water several times (S3) to remove excess anionizing agent. The reactive anionizing agent forms a covalent bond with the fiber and is stuck, so no matter how much it is washed off. There is no restriction on how the fibers are cleaned.

After treating the anionizing agent to the fiber in the same manner as described above, to prepare a dye by dissolving sodium carbonate and yellow wall extraction pigment in a predetermined amount of water (S4).

When the blending ratio of the dye is less than 0.1% by weight of the yellow wall extraction pigment, the color is not sufficiently expressed. If the dyeing ratio exceeds 5% by weight, the color concentration is no longer darkened even when a large amount of dye is used, and the blending ratio of sodium carbonate is 0.1% by weight. If it is less than the dyeing of the yellow wall extract pigments, if it exceeds 1.0% by weight, the dye may decompose to change the color, so 94.0 to 99.9% by weight of water, 0.1 to 1.0% by weight of sodium carbonate and 0.1 to 5.0% by weight of yellow wall extract pigment It is desirable to.

Using the dye prepared as described above, dyeing the fiber prepared in advance (S5), if the dyeing temperature is less than 35 ℃ dyeability is not good, if it exceeds 45 ℃ to increase the manufacturing cost as well as natural dyes The yellow wall extraction pigment may be destroyed and the color may change. If the dyeing time is less than 30 minutes, the dye may not be sufficiently fixed and the productivity will be reduced if it exceeds 50 minutes. It is preferable.

In this case, considering the efficiency of dyeing, the ratio of fibers and dyeing solution is preferably 1: 30, but is not necessarily limited thereto.

The dyed fiber is washed with cold water (S6) and dried (S7) to complete dyeing of the fiber.

Fibers dyed in the same manner as described above have a high saturation and concentration even after the dye has been washed out once in cold water, and the dye is no longer drawn out.

The reactive anionic agent used in the present invention has the following characteristics.

The reactive anionizing agent of the present invention has a reactive group capable of forming a covalent bond with cellulose fibers such as cotton, ramie, burlap, and rayon, and at the same time, an anionic group capable of ionically bonding to berberine, a yellow wall extract pigment having a cation. It is synthesized by having the following reaction scheme.

Synthesis of Reactive Anionic Agents

The reaction type anionizing agent {Sodium4- (4,6-dichloro- [1,3,5] triazin-2-ylamino) -benzenesulfonate} synthesized through the above reaction scheme was obtained through the following reactions. By forming covalent bonds at room temperature and fixing easily, the fiber is easy to process, but does not wash off at all when washed.

Reaction of Reactive Anionizing Agent with Cellulose Fibers

In addition, the anion group of the anion-responsive treatment agent to the cellulose fibers even so, if a responsive anionic agent of the present invention is completely white exerts no effect on the color of the ^dye-in _{(-SO 3 Na <=> -SO3 + Na} +) The yellow wall extraction pigments of the cation are bonded to each other by electrostatic attraction, thereby greatly improving the dyeing amount of the dye.

Hereinafter, the present invention will be described in more detail with reference to preferred embodiments.

(Example 1)

Reactive Anionizing Agent Synthesis

A solution of 0.03 mole (5.7 g) of cyanuric chloride dissolved in 40 ml of acetone was added to water mixed with 90 g of distilled water and 90 g of crushed ice with stirring for 10 minutes, and 0.6 ml of 2N aqueous hydrochloric acid solution was further added. It was added so that it might be pH 1-2. To a cyanuryl chloride dispersion having a pH of 1 to 2, a solution of 0.03 mole (5.20 g) of sulfanilic acid and 0.0016 mole (1.73 g) of sodium carbonate completely dissolved in 48 ml of distilled water was added thereto. It was added to pH 6 and stirred for 60 minutes. After the reaction was completed, the reaction was filtered and washed several times with vacuum filtration and acetone, which was vacuum dried to obtain a reactive anionic agent.

Reactive anionizing agent on cotton fabric

After dissolving 2.0 g of sodium sulfate, 0.2 g of sodium carbonate and 0.1 g of reactive anionic agent in 20 ml of water, add 1 g of cotton fiber to this solution and immerse for 1 hour while maintaining at 35 ° C. to form a covalent bond between the cotton fiber and the reactive anionic agent. The cotton fibers formed with covalent bonds were washed three times in clear water.

Dyeing with Yellow Wall Extract Pigment on Anionized Cotton Fabric

After dissolving 0.05 g of sodium carbonate in 30 ml of water, add 0.2 g of yellow wall extract pigment, dissolve it sufficiently, add 1 g of anionized cotton fabric, dye at 40 ° C. for 40 minutes, wash with cold water, and dry the dyed fiber. Got it.

The comparative example for comparison with the said Example was processed on condition of the following.

(Comparative Example 1)

Cotton fibers that were not treated with anything were dyed with yellow wall extraction pigments in the same manner as in Example 1.

(Comparative Example 2)

Tannin acid solution in which 0.1 g of tannic acid was dissolved in 20 ml of water was treated to cotton fiber in the same manner as in the reactive anionizing agent of Example 1, and the tannin acid-treated cotton fiber was dyed with yellow wall extracting dye in the same manner as in Example 1.

(Comparative Example 3)

Tannin acid solution in which 0.3 g of tannic acid was dissolved in 20 ml of water was treated to cotton fiber in the same manner as in the reactive anionizing agent of Example 1, and the tannin acid-treated cotton fiber was dyed with yellow wall extraction dye in the same manner as in Example 1.

(Comparative Example 4)

The tannin acid solution in which 0.5 g of tannic acid was dissolved in 20 ml of water was treated to cotton fiber in the same manner as in the reactive anionizing agent of Example 1, and the tannin acid-treated cotton fiber was dyed with yellow wall extracting dye in the same manner as in Example 1.

The graph below shows the degree of dyeability increase in the above-described Examples and Comparative Examples by the concentration of dyeing cloth (K / S).

[graph]

Comparison of Derberin's Dyeability in Anionizing and Tannic Acid Treatments

             * Figures in () are ratios to K / S values of Comparative Example 1.

As can be seen in the graph, in Comparative Example 1, in which the cotton fabric which had not been treated with anything was dyed with yellow wall extraction pigment, the K / S value was virtually almost dyed to 0.36, and the treatment was performed with increasing the concentration of tannic acid. The K / S values are 0.78, 1.64, and 1.93, respectively, which are 2.2, 4.6, and 5.4 times higher than those of Comparative Example 1. However, the K / S values of 8.27 were 8.27. It showed 23 times higher value than the case, and it showed that the yellow wall extract dye was very dark by showing K / S value 10 times higher than the case of treatment with the same concentration of tannic acid.

Although the present invention has been described in the above embodiments as described above, it is not necessarily limited thereto, and various modifications may be made without departing from the scope and spirit of the present invention.

As can be clearly seen from the above description, according to the dyeing method of the fiber using the reactive anionizing agent and the yellow wall extracting dye of the present invention, it is shared with the fiber to the fiber which does not have a special anion (-) group such as cotton, ramie, burlap, and rayon. After pre-treatment of the reactive anionizing agent having both a reactive group capable of forming a bond and a yellow wall extraction pigment having a cation (+) and an anionic (-) group capable of ion bonding to form a covalent bond between the fiber and the reactive anionic agent By dyeing the covalently bonded fibers with the yellow wall extraction dye, the fibers have a large number of anion (-) groups, and the yellow wall extraction dye having a cation (+) group is bonded to each other by electrostatic attraction, thereby greatly improving the amount of berberine dyeing. In addition to providing a useful effect such that the dye is not removed even when washed.

1 is a flow chart showing a method for dyeing fibers using the reactive anionizing agent and the yellow wall extracting dye according to the present invention.

Claims (2)

In the dyeing method of the fiber using the yellow wall extraction pigment, 87.5 to 93.3% by weight of water, 5 to 10.0% by weight of sodium sulfate, 0.5 to 1.5% by weight of sodium carbonate, and Sodium 4- (4,6-dichloro- [1,3,5] triazin-2-ylamino) -benzenesulfonate as a reactive anionic agent Dissolving 0.2 to 1.0% by weight (S1); Immersing a predetermined amount of fibers in a dissolved aqueous solution at a temperature in the range of 30 to 40 ° C. for 1 to 2 hours such that a covalent bond is formed between the fibers and the reactive anionizing agent (S2); Washing the fiber in which the covalent bond is formed several times with water (S3); Dissolving 0.1 to 1.0% by weight of sodium carbonate in 94.0 to 99.8% by weight of water, and then dissolving 0.1 to 5.0% by weight of yellow wall extraction pigment to prepare a dye (S4); Dyeing the above-described reactive anionizing agent treated and washed fibers with a prepared dye at a temperature in the range of 35 to 45 ° C. for 30 to 50 minutes (S5); Washing the dyed fibers (S6); And a step of drying the washed fibers (S7). A method of dyeing fibers using a reactive anionizing agent and a yellow wall extract pigment. delete