KR101961189B1 - Dope-dyed Meta-Aramid Fiber having excellent color and Method for producing the same - Google Patents

Abstract

The present invention relates to (S1) a method of forming a meta-aramid dope by dissolving meta-aramid polymerized with M-phenylene diamine (MPD) and isophthaloyl chloride (IPC) ; (S2) diluting the pigment with a polar amide solvent to form a pigment doping; (S3) injecting the pigment dope into a meta-aramid dope to form a meta-aramid-pigment mixture; (S4) injecting the meta-aramid-pigment mixture into meta-aramid dope; And (S5) a step of stirring the mixture after the step (S4), and then spinning the mixture to prepare a crude yarn.

Description

[0001] The present invention relates to a meta-aramid fiber having excellent color and a method for producing the meta-aramid fiber,

The present invention relates to a meta-aramid original adherend and a method of producing the same, and more specifically, to a meta-aramid original adherent having excellent pigment dispersibility and excellent color, and a method for producing the same.

Aramid fiber is a synthetic fiber made from an aromatic polymer that was developed in 1965 with the aim of fiber having strength of fiberglass and heat resistance of asbestos in US Dupont of the United States, . In 1974, the term "aramid" was defined as the general name of "aromatic polyamide in which 85% or more of amide bonds are directly bonded to two aromatic rings" by the Federal Trade Commission, and then ISO-2076, JIS L 0204-2 The name "Edo-aramid" was defined equally.

The aramid is divided into a meta system and a para system by the bonding unit of an amide-bonded aromatic ring. Meta-aramid fibers are excellent in high-temperature heat resistance, and para-aramid fibers have not only high temperature resistance but also high strength and high elasticity.

The meta-aramid is represented by Nomex developed by DuPont, and Conex developed by Dejin. The meta-aramid is a combination of benzene ring and amide group at the meta position. Its strength and elongation are similar to ordinary nylon, but it has very good heat stability. It is light and sweat-absorbing compared to other heat-resistant materials. have. In the early days, the color was limited to a few, but recently it has been made in various colors including fluorescent colors. It is used as fire-resistant clothing, uniforms for racing motorists, astronaut uniforms, work clothes, etc., and for industrial use, it is used for high-temperature filters.

In general, meta-aramids are produced in paper form as well as in fiber and are used in many industrial fields.

The original yarn made from the meta-aramid is dispersed in a meta-aramid polymerized state to prepare a radiation-cured islands. However, the viscosity of the polymer used in the meta-aramid spinning is 200,000 cP or more, which is too high to uniformly disperse the pigment.

Disclosure of Invention Technical Problem [8] The present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to provide a meta-aramid raw material having excellent color by improving the dispersibility of a pigment and a process for producing the same.

It is also intended to improve the productivity by reducing the required amount of pigment required for the same color development.

The present invention relates to (S1) a method of forming a meta-aramid dope by dissolving meta-aramid polymerized with M-phenylene diamine (MPD) and isophthaloyl chloride (IPC) ; (S2) diluting the pigment with a polar amide solvent to form a pigment doping; (S3) injecting the pigment dope into a meta-aramid dope to form a meta-aramid-pigment mixture; (S4) injecting the meta-aramid-pigment mixture into meta-aramid dope; And (S5) a step of stirring the mixture after the step (S4), and then spinning the mixture to prepare a crude yarn.

The present invention relates to a process for preparing an aramid dye having excellent color, wherein the meta-aramid doping in step (S1) is 15 to 25 wt% and the meta-aramid doping in step (S3) is 5 to 15 wt% will be.

The present invention relates to a method for producing an aramid raw material having excellent color, characterized in that the pigment of the meta-aramid-pigment mixture of step (S3) is 25 to 35 wt%.

The present invention relates to a method for producing a meta-aramid original article having excellent color, characterized in that the pigment after the addition is 2 to 10 wt% in the step (S4).

The present invention relates to a method for producing meta-aramid original yarn having excellent coloration, wherein the meta-aramid original yarn has a dyeing concentration (K / S) of 15 to 25.

The present invention relates to a method for producing a meta-aramid original yarn excellent in color, characterized in that the original meta-aramid yarn has a strength of 4.5 to 5.5 g / d.

As described above, the meta-aramid original pigment having excellent color according to the present invention and its production method have the effect of improving the dispersibility of the pigment, facilitating the color development, and reducing the required amount of pigment for the same color development.

In addition, the strength of the fiber can be improved by reducing the content of the pigment.

FIG. 1 is a view showing a step of forming a final polymerized product to produce a meta-aramid raw material having excellent color according to the present invention.
2 is a process diagram for producing a meta-aramid original article having excellent color according to the present invention.

Hereinafter, a preferred embodiment of the present invention will be described in detail. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted so as to avoid obscuring the subject matter of the present invention.

The terms " about ", " substantially ", etc. used to the extent that they are used herein are intended to be taken to mean an approximation of, or approximation to, the numerical values of manufacturing and material tolerances inherent in the meanings mentioned, Accurate or absolute numbers are used to help prevent unauthorized exploitation by unauthorized intruders of the referenced disclosure.

FIG. 1 is a view showing a step of forming a final polymerized product to produce a meta-aramid original article having excellent color according to the present invention, and FIG. 2 is a process diagram for producing a meta-aramid original article having excellent color according to the present invention.

1 and 2, the present invention relates to a process for preparing a polyamide-based polymer comprising the steps of (S1) meta-aramid polymerized with M-phenylene diamine (MPD) and isophthaloyl chloride (IPC) Melting and forming a meta-aramid dope; (S2) diluting the pigment with a polar amide solvent to form a pigment doping; (S3) injecting the pigment dope into a meta-aramid dope to form a meta-aramid-pigment mixture; (S4) injecting the meta-aramid-pigment mixture into meta-aramid dope; And (S5) a step of stirring the mixture after the step (S4), and then spinning the mixture to prepare a crude yarn.

The meta-aramid doping in the step (S1) is preferably 15 to 25 wt%, and the meta-aramid doping in the step (S3) is preferably 5 to 15 wt%. By lowering the concentration of the meta-aramid dope in the step (S3) in which the pigment dope is mixed, the degree of dispersion of the pigment to be added can be increased. If the meta-aramid doping in the step (S3) is performed in the same manner as the meta-aramid doping in the step (S1), there is a problem that the degree of dispersion of the pigment can not be improved and the strength is still lowered. Therefore, it is possible to increase the miscibility by mixing the meta-aramid dope with the relatively low concentration of the pigment, and then to increase the dispersion by mixing with the meta-aramid dope having a relatively high concentration. As the degree of dispersion of the pigment increases, the hue of the color becomes excellent and the hue can be uniformly displayed as a whole. Generally, when the pigment is added, the strength of the fiber is lowered. According to the present invention, the amount of the pigment required to develop the same hue is reduced and the strength of the fiber is accordingly improved.

If the amount of the meta-aramid doped in step (S3) is less than 5 wt%, the concentration of the final mixture becomes low to obtain desired physical properties. When the amount of the meta-aramid doped in step (S3) is higher than 15 wt% Can also be lowered.

The polar amide solvent may be selected from the group consisting of dimethylacetamide (DMAc), N-methylpyrrolidone (NMP), dimethyl formamide (DMF), and dimethyl imidazolidinone Any one of the compounds may be used, and it is preferable to use dimethylacetamide having the most excellent effect.

The pigment in step (S3) is 25 to 35 wt%, and the pigment in step (S4) is 2 to 10 wt%. If the pigment is lower than 25 wt%, the specific gravity of the pigment is lowered overall, and the color development is difficult. If the pigment is higher than 35 wt%, the pigment is relatively more dispersed and the color development may not be uniform. When the pigment of the step (S4) is less than 2 wt%, the color is not only small, but also the concentration of the final mixture to be radiated is low, so that the spinning may be difficult. When the pigment is more than 10 wt%, the color may be sharp, So that uniform color development is difficult and the strength may be lowered.

By controlling the weight ratio of the pigment in steps (S3) and (S4), the pigment can uniformly express the color while maintaining the inherent physical properties of the meta-aramid dope. The pigment may be any one of organic pigments, inorganic pigments, and fluorescent pigments, or a combination thereof. The pigment is preferably an organic synthetic pigment having a high melting point and excellent thermal stability, and a small amount of a dispersing agent may be added to improve dispersibility.

The meta-aramid doping in the step (S4) is the same as the meta-aramid doping in the step (S1), and the meta-aramid doping is preferably 15 to 25 wt%. The viscosity of the meta-aramid dope is controlled according to the mixing ratio of the polar amide solvent and the meta-aramid, and is suitable for radiation when the meta-aramid dope is 15 to 25 wt%. The spinning step is carried out in a coagulating solution by wet spinning and then stretched to produce fibers.

The coagulating solution is a mixture of a polar amide solvent and water. The polar amide solvent is selected from the group consisting of dimethylacetamide (DMAc), N-methylpyrrolidone (NMP), dimethyl formamide (DMF) Dimethylacetamide (DMAc) in an amount of 20 to 60% by weight, water of 40 to 80% by weight, and the like. In the present invention, dimethylacetamide is preferably used, It is preferable to mix them by weight.

Hereinafter, the present invention will be described in more detail with reference to examples. It is to be understood, however, that these examples are provided so as to understand the scope of the present invention, and are not to be construed as limiting the scope of the present invention.

Example  One

Meta-aramid polymerized with M-phenylene diamine (MPD) and isophthaloyl chloride (IPC) was dissolved in dimethylacetamide as a solvent to form a 18 wt% meta-aramid dope. The meta-aramid dope is diluted with dimethylacetamide to 10 wt%. A pigment diluted in dimethylacetamide is added to a 10 wt% meta-aramid dope to produce a meta-aramid-pigment mixture in which 30 wt% pigment is formed. The meta-aramid-pigment mixture was stirred with 18 wt% meta-aramid dope to make the pigment 5 wt%, followed by wet spinning and coagulation to produce the meta-aramid original.

Example  2

Meta-aramid polymerized with M-phenylene diamine (MPD) and isophthaloyl chloride (IPC) was dissolved in dimethylacetamide as a solvent to form a 18 wt% meta-aramid dope. The meta-aramid dope is diluted with dimethylacetamide to 10 wt%. A pigment diluted in dimethylacetamide is added to a 10 wt% meta-aramid dope to produce a meta-aramid-pigment mixture in which 30 wt% pigment is formed. The meta-aramid-pigment mixture was stirred with 18 wt% meta-aramid dope to make the pigment to be 3 wt%, followed by wet spinning and coagulation to produce a meta-aramid original.

Comparative Example  One

Meta-aramid polymerized with M-phenylene diamine (MPD) and isophthaloyl chloride (IPC) was dissolved in dimethylacetamide as a solvent to form a 18 wt% meta-aramid dope. A pigment not diluted in a solvent was added to the 18 wt% meta-aramid dope to prepare a pigment of 5 wt%, followed by stirring. Then, wet-spinning and coagulation were carried out to prepare meta-aramid raw material.

Comparative Example  2

Meta-aramid polymerized with M-phenylene diamine (MPD) and isophthaloyl chloride (IPC) was dissolved in dimethylacetamide as a solvent to form a 18 wt% meta-aramid dope. A pigment diluted with a solvent was added to the 18 wt% meta-aramid dope to form 5 wt% of a pigment, followed by stirring. Then, wet-spinning and coagulation were carried out to prepare meta-aramid raw material.

Comparative Example  3

Meta-aramid polymerized with M-phenylene diamine (MPD) and isophthaloyl chloride (IPC) was dissolved in dimethylacetamide as a solvent and 18 wt% and 10 wt% meta-aramid dope Respectively. A pigment not diluted in a solvent was added to the 10 wt% meta-aramid dope to prepare a meta-aramid-pigment mixture to obtain a pigment of 30 wt%. After that, the pigment was added to 18 wt% meta-aramid dope to form 5 wt% of pigment. The pigment was then stirred and then wet-radiated and coagulated to produce meta-aramid raw material.

◈ Evaluation experiment of examples and comparative examples

Table 1 shows the results of measurement of the concentration and strength of the fibers in the above Examples and Comparative Examples.

* How to measure

(K / S): The surface reflectance was measured at the maximum absorption wavelength of the dyeing fabric using a colorimeter (GretagMacbeth Color-Eye 7000A), and the dyeing concentration (K / S) was calculated according to the Kubelka- To compare the dyeing densities of the dyeing fabrics.

K / S = (1-R) ² / (2R)

(Where K is the extinction coefficient, S is the scattering coefficient, and R is the reflectance)

Strength (g / de): The tensile strength of the fiber is measured using a universal test machine (Instron) according to ASTM D3217.

division Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 Soil concentration (K / S) 23 22 12 14.5 14.8 Strength (g / d) 5.3 5.5 4.1 4.3 4.35

As shown in Table 1, it can be confirmed that the Examples have excellent dyeing concentration as compared with Comparative Examples. It can be confirmed that the dispersibility of the pigment is improved and thus the original yarn having excellent color is produced. In addition, it can be confirmed that, even when the content of the pigment is small, Example 2 has excellent dyeing density and excellent strength, compared with Comparative Example.

Therefore, it is preferable to first disperse the pigment in the relatively low-concentration meta-aramid dope, and then to introduce it into the meta-aramid dope at an appropriate concentration for radiation. When the pigment is added to the relatively low-concentration meta-aramid dope, And then the mixture is preferably introduced. It is preferable to set the weight ratio so as to maintain the inherent physical properties of the meta-aramid without affecting the radiation even with the dilution as in the present invention.

Claims (6)

(S1) A meta-aramid polymerized with M-phenylene diamine (MPD) and isophthaloyl chloride (IPC) was dissolved in a polar amide solvent to prepare a meta-aramid dope of 15 to 25 wt% Dope);
(S2) diluting the pigment with a polar amide solvent to form a pigment doping;
(S3) adding the above pigment doping to a meta-aramid dope at a concentration of 5 to 15 wt% to form a meta-aramid-pigment mixture
(S4) injecting the meta-aramid-pigment mixture into the meta-aramid dope formed in (S1) with a higher meta-aramid concentration; And
(S5) A method of producing a meta-aramid raw material having excellent color, comprising the steps of: (a1) mixing the mixture obtained in step delete The method according to claim 1,
Wherein the meta-aramid-pigment mixture of step (S3) comprises 25 to 35 wt% pigment. The method according to claim 1,
Wherein the pigment in step (S4) is 2 to 10 wt%. The method according to claim 1,
Wherein the meta-aramid original yarn has a dyeing concentration (K / S) of 15 to 25. The method according to claim 1,
Wherein the meta-aramid original yarn has a strength of 4.5 to 5.5 g / d.

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