KR101308009B1 - Nylon knitted goods dying sulfadye and preparing method thereof - Google Patents

Abstract

PURPOSE: A production method of a knitted nylon product which is dyed with a sulfa dye is provided to have an excellent economical value since the process is simple, and to have an excellent wet-color fastness and a rubbing fastness, and to be used appropriately in a product in which a high fastness is required. CONSTITUTION: A production method of a knitted nylon product without gloss which is dyed with a sulfa dyestuff comprises an input step in which a knitted nylon product is placed in the sulfa dyestuff; a step which injects a discharge printing agent under the condition ranged from 45 degree C to 55 degree C; a nylon fabric production step which is dyed with cooling after dying for 30-40 minutes in the elevated temperature ranged from 95-98 degree C; a step which oxidizes the nylon fabric and fixes colors on the nylon fabric which is washed with an aqueous sulfuric acid solution with the concentration ranged 0.03-0.07 percent after washing the knitted nylon product dyed; and a step which cools and washes the knitted nylon product, which is oxidized and colored, with a detergent.

Description

Nylon knitted goods dying sulfadye and Preparing method

The present invention relates to a nylon product dyed with sulfa dyes and a method for manufacturing the same, and to an invention capable of providing a nylon product having high wet fastness and friction fastness.

In general, sulfa dyes are dyes for cotton fibers, dyes that are dyed under an alkali of pH 9 ~ 12.

Nylon was dyed using an acid dye or by reactive dyeing, and the method of dyeing nylon with an acid dye was performed by dyeing at a pH of 4 to 4.5.

Due to the different dyeing conditions, there was no case of dyeing nylon with sulfa dye, and the acid dye itself is difficult to maintain the wet fastness and the friction fastness realistically, so the wet fastness and the friction fastness of the products such as nylon fabric There was a bad problem.

And, in order to improve the dyeability of the nylon fabric, a technique for causing structural change of the nylon fabric using ultraviolet rays, plasma, etc. has been studied, which is very inefficient and increases the manufacturing cost.

Therefore, the present inventors have tried to solve the problem of the method of dyeing nylon with a conventional sulfa dye and the low fastness of nylon products, it was found that it is possible to dye nylon with sulfa dye in a reduced state using a specific dyeing agent, Knowing the optimum amount of use and dyeing conditions to complete the present invention.

The present invention for solving the above problems relates to a nylon knitted fabric dyed with sulfa dye, to provide a nylon knitted fabric dyed with sulfa dyes having a wet fastness of 3.5 to 4.5 grades and a friction fastness of 3-4 grades.

In addition, the present invention relates to a method for producing a nylon knitted fabric dyed with sulfa dye, comprising the steps of adding a sulfa dye to the nylon knit fabric; Inputting a propellant at 45 ° C. to 55 ° C .; Warming up to 95 ° C. to 98 ° C., then dyeing for 30 to 40 minutes and cooling to prepare a dyed nylon knit fabric; Washing the dyed nylon knit fabric, and then oxidizing and coloring the washed nylon knit fabric with a sulfuric acid solution at a concentration of 0.03 to 0.07%; It is to provide a method for producing a nylon fabric dyed with sulfa dyes, including; and a step of cooling and rinsing the oxidized and colored nylon knitted fabric with a cleaning agent at a temperature of 95 ° C.

The manufacturing method of the nylon knitted fabric dyed with sulfa dye of the present invention is simple and excellent in economic efficiency, and the nylon knitted fabric prepared by this method has excellent wet fastness and friction fastness as well as a matt feature, It is suitable for use in products requiring high fastness such as articles and outdoor products.

Hereinafter, the present invention will be described in more detail.

The term "knitting fabric" used in the present invention is made of nylon yarn, and is meant to include various types of concepts such as plain weave, twill weave, satin weave, change weave, change twill weave or change weave weave.

The present invention relates to a nylon knit fabric dyed with sulfa dyes, and the sulfa dyes used in the present invention preferably use sulfone-based reactive dyes, and specifically, sulfur black salt sulfates. Preferably, as the sulfur black, one or more selected from sulfur black 1 and sulfur black 11 may be used alone or in combination.

Sulfur Black 1 is obtained by vulcanization of 2,4-dinitrophenol (2,4-dinitrophenol) with sodium polysulfide, to adjust the vulcanization reaction conditions or as an additive, picric acid (picric acid), peak Picramic acid, dinitrocresol, 2-naphthol, 4′-hydroxy-2,4-dinitrodiphenylamine, etc. It can be manufactured in various grades by adjusting the color and dyeability. In the present invention, the sulfur black 1 may be characterized by including a compound represented by the following Chemical Formula 1.

[Formula 1]

And, the sulfur black 11 is p- (2-naphthylamino) phenol (p- (2-naphthylamino) phenol), phenol (phenol), 4,4'-iminodiphenol (4,4'-iminodiphenol) It is obtained by vulcanization with sodium polysulfide, which controls sulfur reaction conditions or as an additive, picric acid, picramic acid, dinitrocresol, 2-naphthol ), 4'-hydroxy-2,4-dinitrodiphenylamine (4'-hydroxy-2,4-dinitrodiphenylamine) and the like can be prepared in various grades by adjusting the color, dyeability. In the present invention, the sulfur black 11 may be characterized by including a polymer (polymer) of the monomer represented by the following formula (2).

[Formula 2]

In the present invention, the nylon may be used nylon commonly used in the art, it is more preferable to use water-soluble nylon (hydrophilic nylon) than insoluble nylon (non-hydrophilic nylon) in operation.

The nylon knitted fabric of the present invention as described above is dyed by using a sulfa dye, which will be described in detail, incorporating the nylon knitted fabric into a sulfa dye; Injecting the flame retardant, reducing agent and auxiliary agent at 45 ℃ ~ 55 ℃ or less; Warming up to 95 ° C. to 98 ° C., then dyeing for 30 to 40 minutes and cooling to prepare a dyed nylon knit fabric; Washing the dyed nylon knit fabric, and then oxidizing and coloring the washed nylon knit fabric with a sulfuric acid solution at a concentration of 0.03% to 0.07%; And cooling and rinsing the oxidized and colored nylon knit fabric with a cleaning agent.

In addition, in the manufacturing method, the step of refining and deoiling the nylon knitted fabric prior to the step of adding the nylon knitted fabric into the sulfa dye.

And, the nylon knitted fabric and / or sulfa dye may be used the same as described above.

In addition, the sulfa dye is preferably 6 to 18% o.w.f. (On the weight fabric), preferably 8 to 18% for the refined and deoiled nylon knitted fabric, and the sulfa dye is 6% o.w.f. When used below, there may be a problem that the dyeing concentration is lowered, and since the dyeing concentration is no longer increased even when used in excess of 18% owf, there may be a problem of corporate profitability due to the cost increase, so it is used within the above range. It is good.

In addition, the step of adding the flame retardant is added to the sulphate dyeing the nylon woven fabric and refined desulfurization, and then heated up at a temperature increase rate of 1 ℃ / min, 45 ℃ ~ 55 ℃, preferably 48 ℃ ~ 52 ℃ It is better to perform under, but if you put the propellant at less than 45 ℃ may cause problems with the plaque problem and higher the concentration of the propellant, if it exceeds 55 ℃ may have a problem to increase the concentration of the plaque and reducing propellant It is recommended to carry out within the range temperature.

In addition, the flame retardant is used to fix sulfa dyes to nylon fibers, and can be used in the art, and is not particularly limited in the present invention, but preferably Longgalite C (rongalite C, CH ₃ NaO ₃ : NaHSO ₂ CH ₂ O) and NaHSO ₂ CH ₂ O: ₂ H ₂ O It is preferable to use the long gallet C more preferably two or more selected from.

In addition, the flame retardant is 30 to 70 parts by weight, preferably 40 to 60 parts by weight with respect to 100 parts by weight of the sulfa dye, it is preferable to add the propellant to less than 30 parts by weight may have a disadvantage in the dyeing, If the amount of the flame retardant is used in excess of 70 parts by weight, the dyeing of the sulfa dye to the nylon is not very good, there is a problem that the fastness of the nylon knitted fabric may be inferior, it is preferable to use within the above range.

In addition, the detergent may be a non-ionic surfactant, and a cleaner used in the art may be used.

Nylon knitted fabrics dyed with sulfa dyes of the present invention prepared in this manner is wet to (or water) fastness of 3.5 to 4.5 when measured according to the KSK ISO 105-E01 method, and also measured according to the KS K 0650 method. Friction fastness is 3 ~ 4 grade, and it is matt.

EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail based on an Example. However, the scope of the present invention is not limited by the following examples.

[Example]

Example  One

Nylon knitted fabric (trade name: NYLON 40D + SP 20D, manufactured by Huvis) was refined and deoiled to remove impurities and oil from the braid.

Next, 15% o.w.f of sulfa dye (trade name: SULFA BLACK SD, manufactured by CLARIANT raw material) was added to the machine, and the temperature was raised to 50 ° C at a temperature of 1 ° C / min.

Next, 50 parts by weight of Rongalite C (CH ₃ NaO ₃ : NaHSO ₂ CH ₂ O) was added to 100 parts by weight of the sulfa dye as a flame retardant, and then heated to 98 ° C. under 50 ° C., and maintained for 35 minutes.

Next, after cooling and washing, oxidation and color development of the cooled and washed nylon fabric using 0.05% H ₂ SO ₄ aqueous solution was performed, followed by a cleaning agent (non-ion surfactant, trade name: NONION SOAPING ZA, manufacturer Using a Poonglim Emulsifier Tank), after maintaining at 98 ° C. for 10 minutes, a matt nylon fabric dyed with sulfa dye was prepared by cooling with water.

Example  2 to Example  3

In the same manner as in Example 1, but to prepare a nylon knitted fabric dyed with sulfa dye, each of the sulfa dye 6% o.w.f. And 12% o.w.f. Example 2 and Example 3 were implemented.

Example  4 to Example  5

Example 4 was carried out in the same manner as in Example 1, but to prepare a nylon knitted fabric dyed with sulfa dye, so that the temperature is 45 ℃ and 55 ℃ at the time of the application of the dye.

Example  6 ~ Example  7

Example 6 but carried out in the same manner as in Example 1, but to prepare a nylon knitted fabric dyed with sulfa dyes, after the addition of a fluorophore, the temperature was raised to 90 ℃ and 105 ℃, respectively, and maintained for 35 minutes Example 7 was carried out.

Example  8 to Example  9

In the same manner as in Example 1 to prepare a nylon knitted fabric dyed with sulfa dyes, Example 8 and Example 9 were carried out by using a ignition agent 35 parts by weight and 65 parts by weight with respect to 100 parts by weight of the sulfa dyes, respectively. .

Comparative example  1 ~ Comparative example  2

In the same manner as in Example 1, but to prepare a nylon knitted fabric dyed with sulfa dye, each of the sulfa dye 5% o.w.f. And 13% o.w.f. In Comparative Example 1 and Comparative Example 2 were conducted.

Comparative example  3 to Comparative example  4

In the same manner as in Example 1, but to prepare a nylon knitted fabric dyed with sulfa dyes, Comparative Example 3 and Comparative Example 4 was carried out so that the temperature is 40 ℃ and 60 ℃ when the dye is added.

Comparative example  5 ~ Comparative example  6

In the same manner as in Example 1, but to prepare a nylon knitted fabric dyed with sulfa dye, after adding the fluorophore, the temperature was raised to 85 ℃ and 115 ℃, respectively, and maintained for 35 minutes to perform the dyeing Comparative Example 5 and comparison Example 6 was performed.

Comparative example  7 ~ Comparative example  8

In the same manner as in Example 1, but to prepare a nylon knitted fabric dyed with sulfa dye, Comparative Example 7 and Comparative Example 8 was carried out by using a propellant 25 parts by weight and 80 parts by weight with respect to 100 parts by weight of the sulfa dye, respectively. .

Experimental Example

The wet fastness and friction fastness of the nylon knitted fabrics prepared in Examples and Comparative Examples were measured and shown in Table 1 below.

(1) Wet (water) fastness: measured according to KSK ISO 105-E01 method.

(2) Friction fastness: measured according to KS K 0650 method.

division Wet Fastness
(Unit: grade) Friction fastness
(Unit: grade) division Wet Fastness
(Unit: grade) Friction fastness
(Unit: grade) Example 1 4 4 Comparative Example 1 2.5 3 Example 2 3.5 4 Comparative Example 2 4.5 3.5 Example 3 4.5 3.5 Comparative Example 3 4 2.5 Example 4 4 3.5 Comparative Example 4 2.5 3.5 Example 5 3.5 4 Comparative Example 5 2.5 2.5 Example 6 4 4 Comparative Example 6 4 3 Example 7 4 4 Comparative Example 7 2 2.5 Example 8 3.5 3 Comparative Example 8 4.5 3.5 Example 9 4.5 3.5 - - -

Looking at the experimental results of Table 1, in the case of the nylon fabric of the present invention Examples 1 to 9, it was confirmed that the wet fastness is 3.5 ~ 4.5 grade, the friction fastness has a very high fastness as a whole 3 ~ 4 grade .

However, the wet fastness of Comparative Example 1 using sulfa dyes less than 6% o.w.f was less than 3, and in Comparative Example 2, which exceeded 12% o.w.f, there was no improvement in color fastness.

In addition, in the case of Comparative Example 3 in which the temperature of the propellant is less than 45 ℃, compared to Example 4, the friction fastness was not good, in the case of Comparative Example 4 performed at a temperature exceeding 55 ℃, compared with Example 5 When the wet fastness was inferior.

And, in the case of Comparative Example 5 staining at 85 ℃ less than 95 ℃, the fastness overall showed a poor result, in the case of Comparative Example 6 staining at 115 ℃, a temperature exceeding 100 ℃, Example Compared with 7, the friction fastness was lower.

In Comparative Example 7 using less than 30 parts by weight of the flame retardant, the wet fastness and friction fastness was not good, and in Comparative Example 8 exceeding 70 parts by weight, when compared to Example 9, there is no effect of improving the fastness Could confirm.

Through the above experimental example, it was confirmed that the nylon knitted fabric dyed with sulfa dye of the present invention has very good wet fastness and friction fastness. In addition, the nylon fabric dyed with sulfa dye of the present invention is suitable for use in products requiring high fastness such as matt bars, military articles, outdoor products.

Claims (11)

delete delete delete Introducing a nylon knit fabric into sulfa dyes;
Inputting a propellant at 45 ° C. to 55 ° C .;
Warming up to 95 ° C. to 98 ° C., dyeing for 30 minutes to 40 minutes, and then cooling to prepare a dyed nylon fabric;
Washing the dyed nylon knit fabric, and then oxidizing and developing the washed nylon fabric with an aqueous solution of sulfuric acid at a concentration of 0.03 to 0.07%; And
Cooling the oxidized and colored nylon knit fabric with a detergent;
Method for producing a matte nylon knitted fabric dyed with sulfa dye, characterized in that it comprises a. 5. The method of claim 4, further comprising refining and deoiling the nylon fabric prior to the step of introducing the nylon knitted fabric into the sulfa dye. 5. The method of claim 4, wherein the nylon knit fabric comprises water-soluble nylon. The method of claim 4, wherein the sulfa dye
A method for producing a matte nylon knitted fabric dyed with sulfa dye, characterized in that it is used at 6 to 18% owf relative to refined and deoiled nylon knitted fabric. The method of claim 4, wherein the step of adding the propellant
After the sintered and deoiled nylon knitted fabric is put into sulfa dye, the temperature is raised at a temperature increase rate of 1 ° C./min, and then, the nylon knit is dyed with sulfa dye. Way. The method of claim 4, wherein the flame retardant
Matte nylon knitted with a sulfa dye, characterized in that it comprises at least one selected from rongalite C (CH ₃ NaO ₃ : NaHSO ₂ CH ₂ O) and NaHSO ₂ CH ₂ O: 2H ₂ O. Manufacturing method. The method of claim 4, wherein the propellant of the step of adding a propellant
Method for producing a matte nylon knitted fabric dyed with sulfa dye, characterized in that the input to 30 to 70 parts by weight based on 100 parts by weight of the sulfa dye. The method of claim 4, wherein the cleaning agent is a nonionic surfactant.