KR20190017148A - Two bath dyeing method for modacrylic/meta-aramid/cotton blended fibers - Google Patents

Abstract

The present invention relates to a method for two bath dyeing of modacrylic/meta-aramid/cotton blended fibers. The method of the present invention comprises the steps of: increasing the temperature of a first dyeing solution in which benzyl alcohol, nonionic arylether or acetophenone-based swelling agent, acetic acid, cationic dyes, sodium nitrate and water are mixed, primarily dyeing the modacrylic/meta-aramid/cotton blended fibers with the first dyeing solution at 120 to 130°C, and cooling the modacrylic/meta-aramid/cotton blended fibers dyed with the first dyeing solution to obtain primarily dyed blended fibers; cleaning the primarily dyed blended fibers with an aqueous solution, to which sodium hydrosulfite and sodium carbonate are added, to obtain cleaned blended fibers; and increasing the temperature of a second dyeing solution, in which sodium sulfate, reactive dyes, soda ash and water are mixed, to 60 to 80°C, secondly dyeing the cleaned blended fibers with the second dyeing solution, and cooling and washing secondly dyed blended fibers. As described above, the dyeing method of the present invention can dye meta-aramid, modacrylic and cotton fibers in dark colors without lowering color fastness, and can perform a mass production process even without additional production facilities. Further, the dyeing method can minimize an economic burden by blending a meta-aramid fiber with modacrylic and cotton fibers while having flame resistance of the meta-aramid fiber.

Description

META-ARAMID / COTTON BLENDED FIBERS METOD FOR MODACRYLIC / META-ARAMID / COTTON BLENDED FIBERS [0002]

The present invention relates to a two-bath dyeing method of modacrylic / meta-based aramid / cotton blend fibers. In particular, the present invention relates to a method for dyeing a modacrylic / The present invention relates to a dyeing method capable of dyeing using a reactive dye.

Meta-based aramid fiber has excellent chemical resistance and heat resistance and is widely used as flame retardant protective material. Fireproof fabric for protection of the human body in extreme situations like fire brigade is a typical example.

However, the use of meta-based aramid fibers alone is not suitable for industrial flame retardant workwear products, which have to be worn by a large number of workers due to their high price. Modacrylic and cotton fibers are blended with meta-based aramid to exhibit flame retardancy at reasonable prices.

The cationic dyes used in modacrylite dyeing have the property that the dyeing is smooth at pH 2 ~ 6, which is an acidic bath.

On the other hand, the meta-based aramid is also stained in an acidic bath having a pH of 2 to 6 by using a cationic dye, but when the swelling agent is not used, it is not a normal physical / chemical bond between the cationic dye and the fiber, It is not only a cause of deterioration but also makes it difficult to dye in a thick color.

In order to overcome this problem, there is an original yarn which is a fiber having a unique color by adding pigment at the stage of manufacturing meta-system aramid fiber.

Korean Patent Laid-Open Publication No. 10-2013-0133348 discloses a continuous aramid short fiber having a gray or black color in a short length of aramid staple fibers, which is obtained by using a gray or black coloring material, and a method for producing the same.

However, there is a problem that it is difficult to quickly meet the needs of consumers who want various colors because the types of colors are not varied and the production amount is limited.

Disclosure of the Invention The present invention overcomes the above-mentioned problems of the prior art and overcomes the problems of the conventional dyeing method and cationic dyeing method, thereby enabling dyeing of two baths capable of securing high color tone without lowering the fastness of the meta-based aramid fibers , And to provide a dyeing method capable of mass production without the need for additional production facilities.

In order to solve the above technical problems, the inventors of the present invention have found that when the cationic dye dyeing method and the additives such as benzyl alcohol, nonionic aryl ether, and acetophenone swelling agent are used together, the modacrylic / The present inventors have completed the present invention by deriving a two-bath dyeing method capable of dyeing a cotton fiber using an additive such as a reactive dye, a neutral salt, and an alkali preparation.

In order to accomplish the above object, the two-bath dyeing method of modacryl / meta-based aramid / cotton blend fibers according to an embodiment of the present invention is characterized in that modacrylic / meta aramid / cotton blend fibers are mixed with benzyl alcohol or non- Or a primary dye mixed with an acetophenone-based swelling agent, acetic acid, a cationic dye, sodium nitrate and water, heating the primary dye at 120 to 130 ° C and cooling; Washing said primary stained blend fibers in an aqueous solution to which sodium hydrosulfite and sodium carbonate have been added; And a step of raising the temperature of the washed blended fibers to 60 to 80 캜 by mixing sodium sulfate, a reactive dye, soda ash and water, and then dyeing the washed dye, cooling, and washing.

Preferably, the primary dyeing step is a step of adding a modacrylic / meta-based compound to an aqueous solution containing 1 to 5 g / l of acetic acid and 5 to 50 g / l of a swelling agent selected from benzyl alcohol, nonionic aryl ether or acetophenone- Treating the aramid / cotton blend fibers at 60 to 70 DEG C for 10 to 20 minutes; Adding 0.001-30 wt% of a cationic dye to the mixture at 60-70 캜 for 10-15 min; Adding 10 to 30 g / l of sodium nitrate at 60 to 70 占 폚 for 2 to 3 times in 30 minutes; And a step of raising the temperature to 120 to 130 캜, dying the mixture for 40 to 90 minutes, cooling to 60 to 70 캜 and washing with water.

Preferably, the washing step is a step of washing with an aqueous solution containing 0.5 to 3 g / l of sodium hydrosulfite and 0.5 to 3 g / l of sodium carbonate at 60 캜 for 20 minutes and further washing with water.

Preferably, in the secondary dyeing step, the primary dyed fabric is dipped in an aqueous solution to which 0.001-30 fiber weight% of reactive dye, 15-100 g / l sodium sulfate and 5-20 g / l sodium carbonate are added, Lt; 0 > C for 30 to 60 minutes, and washing and soaking.

According to the present invention, meta-based aramid, modacrylic, and cotton fibers can be dyed in a high color without deterioration of fastness, and a method of mass-production without mass production can be provided.

In addition, while having flame retardancy of meta-based aramid fibers, they can mix with modacrylic and cotton fibers to minimize the economic burden.

1 is a graph comparing color intensities of a primary stained modacryl / meta based aramid / cotton blend fiber according to an embodiment of the present invention.
Figure 2 is a photograph of the primary stained modacrylic / meta-based aramid / cotton blend fabric of Figure 1;

Exemplary embodiments of the present invention will be described below with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention. In the drawings and specification, there are shown in the drawings and will not be described in detail, and only the technical features related to the present invention are shown or described only briefly. Respectively. The specific configurations and functions described in detail herein are not intended to be limiting, but merely as the basis for the claims and as a basis for teaching the ordinary skill in the art to which the present invention pertains in various ways.

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

The present invention relates to a process for producing a water-based blend of modacrylic / meta-based aramid / cotton blend fibers immersed in an aqueous solution containing 1 to 5 g / l of acetic acid and 5 to 50 g / l of benzyl alcohol or nonionic aryl ether or acetophenone- Treated for 10 to 20 minutes, treated at 60 to 70 ° C for 10 to 15 minutes with 0.001 to 30 wt% of a cationic dye added thereto, and 10 to 30 g / l of sodium nitrate was added to the resulting solution at 60 to 70 ° C for 30 minutes for several times After the addition, the temperature is raised to 120 to 130 ° C, and the mixture is dyed for 40 to 90 minutes, cooled to 60 to 70 ° C and washed with water. The washed cloth is washed with an aqueous solution containing 0.5 to 3 g / l of sodium hydrosulfite and 0.5 to 3 g / l of sodium carbonate at 60 ° C for 20 minutes and rinsed again.

The primary dyed fabric was immersed in an aqueous solution containing 0.001-30 weight% of a reactive dye, 15-100 g / l of sodium sulfate, and 5-20 g / l of sodium carbonate, Dyed, washed and soaped.

First, the salt solution used in the primary staining of the present invention is an aqueous solution containing benzyl alcohol or a nonionic aryl ether or an acetophenone based swelling agent. By containing a swelling agent, the molecular structure of the rigid meta-based aramid can be loosely And allows the cationic dye to be easily stained with meta-based aramid fibers.

In addition, sodium nitrate is required to adjust the solubility of the dye in an aqueous solution so that the dye is easily accessible to the fibers, and dissolves in the salt solution several times at intervals of 10 minutes or more. This is because if sodium nitrate is used in large amounts at one time, the dye will settle and result in uneven dyeing, such as spots on the fiber.

In the present invention, the reason why the modacrylic / meta-based aramid fiber portion is firstly colored and the cotton fiber portion is secondarily colored is as follows.

When cotton fibers are stained with reactive dyes at 60 to 80 ° C and then modacrylic / meta-based aramid stains at temperatures of 120 to 130 ° C, which is higher than 60 to 80 ° C, the dyeing of cotton fibers is discolored, .

In addition, since the swelling agent used in the meta-based aramid dyeing has a swelling effect on almost all the fibers although the effect is different in size, the cationic dye can be a simple dye, not a physical / chemical bond to the cotton fiber, Causing difficulty in dyeing the same color between the modacrylic / meta-based aramid and cotton fibers.

In addition, sodium hydrosulfite is used for cleaning after dyeing of modacrylic / meta-based aramid fibers, dyeing cotton fibers and dyeing modacrylic / meta-based aramids followed by washing with sodium hydrosulfite, In addition to removing undyed dyes from modacrylic / meta-based aramid fibers, it also affects dyes dyed on cotton fibers, which may cause discoloration of cotton fiber portions.

Therefore, in the present invention, the modacryl / meta-based aramid / cotton fiber is immersed in an aqueous solution containing 1 to 5 g / l of acetic acid and 5 to 50 g / l of benzyl alcohol or nonionic aryl ether or acetophenone swelling agent at 60 to 70 ° C Treated for 10 to 20 minutes, treated at 60 to 70 ° C for 10 to 15 minutes with 0.001 to 30 wt% of a cationic dye added thereto, and 10 to 30 g / l of sodium nitrate was added to the resulting solution at 60 to 70 ° C for 30 minutes for several times After the addition, the temperature is raised to 120 to 130 ° C., and the modacrylic / meta-based aramid fiber portion is firstly dyed for 40 to 90 minutes, cooled to 60 to 70 ° C. and washed with water. The washed cloth is washed with an aqueous solution containing 0.5 to 3 g / l of sodium hydrosulfite and 0.5 to 3 g / l of sodium carbonate at 60 ° C for 20 minutes and rinsed again.

After the first dyeing, 0.001-30 fiber weight of the reactive dye and 15-100 g / l of sodium sulfate are treated at 25-50 ° C for 10-30 minutes, sodium carbonate 5-20 g / The temperature is elevated, and secondary dyeing is performed for 30 to 60 minutes, and washing and soaking are carried out to complete the dyeing process.

The weight ratio of the modacrylic / meta-based aramid / cotton blend fibers is preferably in the order of cotton, modacryl, and meta-aramid in the order of flame retardancy, and in terms of economy, the weight is preferably increased in the order of meta-based aramid, modacryl and cotton Do.

The following examples illustrate non-limiting examples of the two-bath dyeing method of the modacrylic / meta-based aramid / cotton blend fibers of the present invention.

[Example 1]

Modacrylic (38%) / meta-based aramid (30%) / cotton (32%) blend fibers were immersed in an aqueous solution containing 2 g / l of acetic acid and 0, 5, 10, 15, 30 and 50 g / Treated at 60 DEG C for 15 minutes, treated with 60 weight% of catechin dye (Doracryl BLACK MD) at 60 DEG C for 10 minutes, and 20 g / l of sodium nitrate was added in two portions at 60 DEG C for 30 minutes, The temperature is raised to 120 ° C, and the mixture is dyed for 60 minutes, cooled to 60 ° C and washed with water. The washed fabric was washed with an aqueous solution containing 2 g / l of sodium hydrosulfite and 2 g / l of sodium carbonate at 60 캜 for 20 minutes, and further washed with water to complete primary staining.

The primary dyed fabric was dipped in an aqueous solution containing 2% by weight of a reactive dye (Remazol D / BLACK GWF), 50 g / l of sodium sulfate and 13 g / l of sodium carbonate, and then secondary dyed at 80 캜 for 40 minutes. Lt; RTI ID = 0.0 > C, < / RTI >

[Example 2]

(38%) / meta-based aramid (30%) / cotton (32%) blend fibers were added to an aqueous solution containing 2 g / l of acetic acid and 0, 5, 10, 15, 30 and 50 g / Treated at 60 ° C for 15 minutes, treated with 60% by weight of catechin dye (Doracryl BLACK MD) at 60 ° C for 10 minutes, and 20 g / l of sodium nitrate was added in two portions at 60 ° C for 30 minutes After that, the temperature was raised to 120 캜, stained for 60 minutes, cooled to 60 캜 and washed with water. The washed fabric was washed with an aqueous solution containing 2 g / l of sodium hydrosulfite and 2 g / l of sodium carbonate at 60 캜 for 20 minutes, and further washed with water to complete primary staining.

The primary dyed fabric was dipped in an aqueous solution containing 2 wt% of a reactive dye (Remazol D / BLACK GWF), 50 g / l of sodium sulfate and 13 g / l of sodium carbonate, and then secondary dyed at 80 캜 for 40 minutes. Lt; RTI ID = 0.0 > C, < / RTI >

The color intensity of the primary stained fabric was measured by the above examples and is shown in Table 1 below.

Swelling agent concentration
(g / l) Total K / S ^One)  Growth rate ( % ) Example 1 Example 2 5 4 12 10 11 34 15 15 47 30 30 101 50 52 108

1) The K / S value representing the apparent concentration value was calculated using the Kubelka-Munk equation (1) after measuring the reflectance of short wavelength at 10 nm intervals in the visible light wavelength range (360 to 750 nm) using a colorimeter, The color intensity was compared with the total K / S value of the short wavelength K / S of the interval.

……… 식(1)

... ... ... Equation (1)

K: absorption coefficient

S: scattering coefficient

R: reflectance

According to the present invention, meta-based aramid, modacrylic, and cotton fibers can be dyed in a high color without deterioration of fastness, and a method of mass-production without mass production can be provided.

In addition, it has flame retardancy of meta-based aramid fiber, but it can mix with modacrylite and cotton fiber to minimize economic burden.

Although several embodiments of the present invention have been described, these embodiments are presented by way of example and are not intended to limit the scope of the invention. These new embodiments can be implemented in various other forms, and various omissions, substitutions, and alterations can be made without departing from the gist of the invention. These embodiments and their modifications are included in the scope and spirit of the invention, and are included in the scope of the invention described in claims and their equivalents.

Claims (4)

The modacrylic / meta-aramid / cotton blend fibers are heated to a temperature of 120 to 130 ° C at a temperature of from 120 to 130 ° C to form a primary dye mixed with benzyl alcohol or a nonionic aryl ether or acetophenone type swelling agent, acetic acid, cationic dye, sodium nitrate, Dyeing and cooling;
Washing said primary stained blend fibers in an aqueous solution to which sodium hydrosulfite and sodium carbonate have been added; And
And washing the washed blended fibers with sodium sulphate, reactive dye, secondary dye mixed with soda ash and water to a temperature of 60 to 80 캜 for secondary dyeing, followed by cooling and washing with water. / Meta system aramid / cotton blend fiber 2 way dyeing method. The method according to claim 1,
In the primary dyeing step,
The modacrylic / meta-based aramid / cotton blend fibers were immersed in an aqueous solution containing 1 to 5 g / l of acetic acid and 5 to 50 g / l of a swelling agent of benzyl alcohol, nonionic aryl ether or acetophenone, Lt; 0 > C for 10 to 20 minutes;
Adding 0.001-30 wt% of a cationic dye to the mixture at 60-70 캜 for 10-15 min;
Adding 10 to 30 g / l of sodium nitrate at 60 to 70 占 폚 for 2 to 3 times in 30 minutes; And
A step of raising the temperature to 120 to 130 캜, dying for 40 to 90 minutes, and cooling to 60 to 70 캜, followed by washing with water, followed by two-bath dyeing of the modacrylic / meta-based aramid / cotton blend fiber. The method according to claim 1,
Wherein the step of washing is a step of washing with an aqueous solution containing 0.5 to 3 g / l of sodium hydrosulfite and 0.5 to 3 g / l of sodium carbonate for 20 minutes at 60 ° C and further washing with water. The modacrylic / meta-based aramid / cotton blend Two-bath dyeing method of fiber. The method according to claim 1,
In the secondary dyeing step, the primary dyed fabric is dipped in an aqueous solution to which 0.001-30 weight% of a reactive dye, 15-100 g / l of sodium sulfate and 5-20 g / l of sodium carbonate are added, A second dyeing for 60 minutes, followed by washing and soaking. The two-bath dyeing method of modacryl / meta-based aramid / cotton blend fibers.

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