KR20120077239A - Meta aramid staple fiber dyeing evaluation method - Google Patents

Abstract

PURPOSE: A method for evaluating dyeing property of meta aramid staple fibers is provided to quickly evaluate colors. CONSTITUTION: A method for evaluating dyeing property of meta aramid staple fibers comprises: a step of dipping the meta aramid staple fibers in a refining solution containing 0.5-3 wt% of water solution; a step of dyeing the meta aramid staple fibers in a solution containing 20-40 g/L of acetophenone and 0.5-20% of C.I basic alkaline dye; a step of dipping the dyed meta aramid staple fibers in a reducing solution containing 0.5-1.5% of soda ash; a step of washing the staple fibers with water and drying; and a step of evaluating the dyeing property.

Description

Dyeing evaluation method of meta aramid short fibers {META ARAMID STAPLE FIBER DYEING EVALUATION METHOD}

The present invention relates to a method for evaluating the dyeability of meta aramid short fibers, and relates to a method for evaluating the dyeability of meta aramid short fibers by carrying out carrier dyeing of meta aramid short fibers in a short time.

Aramid is a general term for Aromatic Polyamide fibers, and is composed of long chain-shaped synthetic polyamides composed of fibers. At least 85% of the amide bonds are artificial fibers directly attached to two aromatic rings. Para-Aramid fibers and Meta-Aramid fibers are largely divided, and Para-Aramid is divided into Polymer and Copolymer. Para-based has high strength and high modulus, and meta-based has thermal stability It is excellent.

The meta aramid is polycondensed with aromatic diamine and aromatic diacid chloride and is commercially available under the trade name Nomex. In addition, p-phenylenediamine and 3,4'- are added to terephthalic acid chloride. A polyaromatic etheramide was developed in Teijin by reacting diaminophenyl ether to make a polymer, wet spinning it, and stretching it to orient the crystal.

The meta-aramid fibers are manufactured in filament yarns or spun yarns because of their excellent heat resistance and flame retardancy, and are widely used in protective clothing such as electrical parts materials such as electrical insulation materials and fire fighting suits. Various research and development has been done so far.

The conventional meta-aramid short fibers were dyed by the method of weaving, dyeing, dyeing in a yarn state, pretreatment, and dyeing.

In the case of dyeing with ombre as described above, as shown in FIG. As shown in Fig. 2, dyeing was performed by spinning, canning, sizing, weaving, pretreatment, post-treatment, reduction, and washing and drying.

As described above, the dyeability evaluation method of the conventional meta-aramid short fibers requires a long time for dyeing and evaluation, which makes it difficult to evaluate the dyeability of various dyes.

The present invention has been invented to solve the above problems, and an object of the present invention is to improve the dyeability evaluation method of meta-aramid short fibers to dye the short fibers by carrier dyeing to evaluate the dyeability.

Moreover, it aims at improving the dyeability evaluation method of the meta aramid short fiber which can evaluate the dyeability of the meta aramid short fiber by the very small amount of the meta aramid short fiber.

The present invention is a method for evaluating the dyeability of meta aramid short fibers, comprising: a refining step of immersing the meta aramid short fibers in a refining solution, which is an aqueous solution of soda ash (0.5 to 3.0%), for refining and washing with water; A dyeing step of dyeing the refined meta-aramid short fibers in a salt bath of 20 to 40 g / L of acetophenone, a carrier, and 0.5 to 20% of an aqueous basic dye of C.I Basic; A reduction step of reducing the dyed meta-aramid short fibers by immersing the short fibers in a reducing solution which is an aqueous solution of 0.5 to 1.5% of soda ash; Water washing and drying step of washing the reduced meta-aramid short fibers with water and drying; And a dyeability evaluation process of evaluating the dyeability of the dried meta-aramid short fibers.

The present invention also provides a method for evaluating the dyeability of meta-aramid short fibers, which is performed before the refining step.

In addition, the refining process provides a method for assessing the dyeability of meta-aramid short fibers, characterized in that the short fibers are immersed in the refining solution at 70 ~ 100 ℃ 30 to 80 minutes to be refined.

In addition, the dyeing process provides a method for evaluating the dyeability of meta-aramid short fibers, characterized in that the short fibers are immersed in a dye bath at 100 ~ 150 ℃ 30 to 100 minutes to dye.

The present invention also provides a method for evaluating the dyeability of meta-aramid short fibers, which further comprises adding 0.3 to 0.7 g / l of alkyl ethoxylate-based homogenizer and 15 to 30 g / l of sodium nitrate for uniform dyeing in the dyeing process. .

In addition, the pH of the dye bath in the dyeing process provides a method for assessing the dyeability of meta-aramid short fibers, characterized in that 2 to 5.

In addition, the reduction process provides a method for assessing the dyeability of meta-aramid short fibers, characterized in that the short fibers are immersed in the refining solution at 70 to 100 minutes for 15 to 80 minutes to reduce.

In addition, the meta aramid short fibers provides a method for evaluating the dyeability of meta aramid short fibers, characterized in that using 3 ~ 10g.

In addition, the dyeability evaluation process provides a method for evaluating the dyeability of meta-aramid short fibers characterized in that the color difference L value of 90 to 99, the dyeing ratio of 90 to 99% of the same standard dye is compared and evaluated.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. First, it should be noted that, in the drawings, the same components or parts have the same reference numerals as much as possible. In describing the present invention, detailed descriptions of related well-known functions or configurations are omitted in order not to obscure the subject matter of the present invention.

As used herein, the terms "about", "substantially", and the like, are used at, or in close proximity to, numerical values when manufacturing and material tolerances inherent in the meanings indicated are intended to aid the understanding of the invention. Accurate or absolute figures are used to assist in the prevention of unfair use by unscrupulous infringers.

The present invention relates to a dyeability evaluation method of the meta-aramid short fibers as shown in FIG.

In order to improve the dyeability of the meta-aramid short fibers and to accurately evaluate the dyeability, it is preferable to perform a carding process before the refining process.

The carding process is a process of combing the meta-aramid short fibers uniformly in the longitudinal direction of the fiber with a brush needle like a carding process of spinning to form a web to improve the dyeability by preventing the short fibers from tangling during dyeing.

The fineness of the meta-aramid short fibers which can be evaluated by the meta-aramid short-fiber dyeability evaluation method of the present invention is not limited in length, but when the meta-aramid short fibers are too large and the length is too long, the dyeing is not uniformly evaluated. It may be difficult to evaluate the meta-aramid short fibers having a length of 10 to 100 mm of 0.5 to 5 denier (Denier).

In addition, if the amount of the meta-aramid short fibers to be evaluated is too small, the evaluation may not be made properly, the meta-aramid short fibers are preferably dyed more than 3g to evaluate, more preferably the meta-aramid short fibers 3 ~ 10g Is to use

In the refining process, the meta-aramid short fibers are immersed in a refining solution, which is an aqueous solution of soda ash 0.5-3.0%, to remove impurities contained in the fibers during spinning or moving before dyeing, and the refining solution for the next dyeing process. It is a process washing with water to remove.

In the refining step, the meta-aramid short fibers are preferably immersed in the refining solution at 70 to 100 ° C for 30 to 80 minutes, and the water washing is preferably washed with water at 60 to 95 ° C.

The dyeing process is a step of dyeing the refined meta-aramid short fibers in a salt bath of 20 ~ 40g / ℓ of carrier (acetophenone), a basic dye 0.5 ~ 20% of CI Basic (CI Basic) Acetophenone, a carrier, swells the meta aramid short fibers to dye the basic dye of CI Basic into the molecules of the meta aramid to dye the meta aramid short fibers.

In the dyeing step, it is preferable that the meta-aramid short fibers are immersed in a dye bath at 100-150 ° C. for 30-100 minutes for dyeing.

In the dyeing process, 0.3 to 0.7 g / l of alkyl ethoxylate leveling agent may be used as a leveling agent for uniform dyeing, and may be increased by further adding 15-30 g / l of sodium nitrate as a dye dissolving agent. .

In addition, the pH of the salt bath in the dyeing step is preferably 2-5. Glacial acetic acid may be further added to adjust the pH of the salt bath. The glacial acetic acid will preferably be added in an appropriate amount depending on the desired pH.

The reducing process is to reduce the dyed meta-aramid short fibers dyed in acid-based salt solution by reducing the dyed meta aramid short fibers by dipping the short fibers in a reducing solution of soda ash 0.5-1.5% aqueous solution, dyeing It is a process to remove dyes from meta-aramid short fibers.

In the reduction step, it is preferable that the meta-aramid short fibers are immersed in a refining solution at 70-100 ° C. for 15 to 80 minutes to be reduced.

In the washing and drying step, the reduced meta-aramid short fibers are washed with water and dried, and the washing with water is preferably washed with water at 60 to 90 ° C.

The drying may be a high temperature or low temperature drying, but it may be preferable to dry with hot air of 50 ~ 200 ℃ for the speed of the process.

Staining of the meta-aramid short fibers described above may be performed sequentially in one bath.

In the dyeing evaluation process of the meta-aramid short fibers dyed as described above, it would be preferable to compare and evaluate the same staining standard surface.

The standard surface may be a synthetic resin such as aramid-based, polyamide-based, polyester-based having a color difference L value of 90 to 99, the dyeing ratio of the dye to 90 to 99%.

The meta-aramid short-fiber dyeing evaluation method according to the present invention described above is an evaluation method for carrier dyeing a fibrous material having a limited length in a short time, the preliminary dyeing to the actual state by spinning the yarn and pre-treatment after weaving it is mainly It is effective in evaluating the staining of metaaramid short fiber by breaking away from the dyeing evaluation.

In addition, by using a small amount of meta-aramid short fibers, all processes can be performed in one bath (bath), there is an effect that can evaluate the meta-aramid short-fiber dyeing by a simple method.

1 is a meta-aramid dyeability evaluation process according to the prior art ombre.
Figure 2 is a meta aramid dyeability evaluation process according to the prior art after dyeing.
Figure 3 is a meta aramid dyeability evaluation process according to the present invention.

Hereinafter, although the Example of the dyeing | stainability evaluation method of the meta aramid short fiber of this invention is shown, it is not limited.

Example 1

The meta-aramid short fibers of 2.0 denia 51mm were opened, and 5 g of them were collected. As a standard surface, polyester short fibers having a color difference L value of 95% and a dyeing ratio of 95% or more were used as standard surfaces.

The meta-aramid short fibers and standard cotton were immersed in 0.5% by weight of soda ash at 65-70 ° C., refined for 60 minutes, and washed with water.

The refined meta-aramid short fibers and the standard cotton were 20% CI Basic mix`Black XBLNS Liq`, which is a basic dye of CI Basic, 0.5g / l of an alkyl ethoxylate system as a leveling agent, and 30g / of acetophenone as a carrier. The dyeing was carried out for 30 minutes in a salt bath of 135 ° C. which was an aqueous solution of 20 g / L of sodium nitrate as a dye dissolving agent. The salt bath was adjusted to pH 3.5 with glacial acetic acid.

The dyed meta-aramid short fibers and standard cotton were immersed in a reducing solution, which is an aqueous solution of soda ash 1.5% for 15 minutes, reduced, washed with water, and dried.

L value and salt difference were evaluated using the color difference meter which evaluated the dyeability of the dried meta aramid short fibers and the standard cotton.

The color difference meter is set by measuring the L value of Example 1 after adjusting the '0' point (Lab) of the color difference meter with the model name Color-Eye 7000A, X-rite Serial Number = IN2584309983, and the light source D65-10 (daylight-Neutal). One value was averaged and the salt difference was calculated from the L value of the standard surface.

division L value Salt tea (%) Standard cotton 14.12 - Example 1 14.32 98.60335196

Example 2

5 g of the aramid short fibers of 1.5-denia 38mm meta-aramid were opened, and the polyester short fibers having a color difference L value of 95% and a dyeing ratio of 95% or more were used as standard surfaces.

The meta-aramid short fibers and standard cotton were immersed in 0.5% by weight of soda ash at 90-95 ° C., refined for 60 minutes, and washed with water.

The refined meta-aramid short fibers and standard cotton were CI Basic Red 29 0.5%, which is a basic dye of CI Basic, alkyl ethoxylate-based 0.5g / l as a leveling agent, acetophenone 30g / L as a carrier, and a dye dissolving agent. It was dyed for 90 minutes in a salt bath of 110 ° C. which was an aqueous solution of 20 g / L of phosphorus sodium nitrate. The salt bath was adjusted to pH 3.5 with glacial acetic acid.

The dyed meta-aramid short fibers and standard cotton were immersed in a reducing solution, which is an aqueous solution of soda ash 0.1% for 15 minutes, reduced, washed with water, and dried.

L value and salt difference were evaluated using the color difference meter which evaluated the dyeability of the dried meta aramid short fibers and the standard cotton.

The color difference meter is measured by measuring L value in Example 2 after setting '0' point (Lab) of the color difference meter with model name Color-Eye 7000A, X-rite Serial Number = IN2584309983, and light source D65-10 (daylight-Neutal). One value was averaged and the salt difference was calculated from the L value of the standard surface.

division L value Salt tea (%) Standard cotton 38.07 - Example 2 38.46 98.98595944

Example 3

1.0 g of 38 mm meta-aramid short fiber was opened and 5 g of them were collected. As standard surface, polyester short fiber having 95% brightness of color difference L value and 95% of dyeing ratio is used as standard surface.

The meta-aramid short fibers and standard cotton were immersed in 1.5% by weight of soda ash at 80 to 85 ° C, refined for 45 minutes, and washed with water.

The refined meta-aramid short fibers and standard cotton were CI Basic blue 53 10.0%, which is a basic dye of CI Basic, alkyl ethoxylate-based 0.5g / L as a leveling agent, acetophenone as a carrier 30g / L, dye dissolving agent It was dyed for 60 minutes at 125 ° C. in a salt bath which was an aqueous solution of 20 g / L of phosphorus sodium nitrate. The salt bath was adjusted to pH 3.5 with glacial acetic acid.

The dyed meta-aramid short fibers and standard cotton were immersed in a reducing solution, which is an aqueous solution of 1.0% soda ash for 15 minutes, reduced, washed with water, and dried.

L value and salt difference were evaluated using the color difference meter which evaluated the dyeability of the dried meta aramid short fibers and the standard cotton.

The color difference meter is measured by measuring L value in Example 3 after setting '0' point (Lab) of the color difference meter with model name Color-Eye 7000A, X-rite Serial Number = IN2584309983, and light source D65-10 (daylight-Neutal). One value was averaged and the salt difference was calculated from the L value of the standard surface.

division L value Salt tea (%) Standard cotton 28.52 - Sample face 1 28.84 98.89042996

Example 4

0.8 g of 38 mm meta-aramid short fibers were opened and 5 g of them were collected. As standard surfaces, polyester short fibers having 95% lightness of the color difference L value and 95% or more of dyeing ratio were used as standard surfaces.

The meta-aramid short fibers and standard cotton were immersed in 0.5% by weight of soda ash at 90-95 ° C., refined for 30 minutes, and washed with water.

The refined meta-aramid short fibers and standard cotton were CI Basic Orange 22 15.0%, a basic dye of CI Basic, alkyl ethoxylate-based 0.5g / L as a leveling agent, acetophenone as a carrier 30g / L, dye dissolving agent It was dyed for 90 minutes in a salt bath of 165 ° C. which was an aqueous solution of 20 g / L of phosphorus sodium nitrate. The salt bath was adjusted to pH 3.5 with glacial acetic acid.

The dyed meta-aramid short fibers and standard cotton were immersed in a reducing solution, which is an aqueous solution of soda ash 1.5% for 15 minutes, reduced, washed with water, and dried.

L value and salt difference were evaluated using the color difference meter which evaluated the dyeability of the dried meta aramid short fibers and the standard cotton.

The color difference meter is measured by measuring L value for Example 4 after setting '0' point (Lab) of the color difference meter with model name Color-Eye 7000A, X-rite Serial Number = IN2584309983, and light source D65-10 (daylight-Neutal). One value was averaged and the salt difference was calculated from the L value of the standard surface.

division L value Salt tea (%) Standard cotton 51.47 - Example 4 51.63 99.69010265

As shown in Examples 1 to 4, the meta-aramid short fiber dyeability evaluation method according to the present invention can easily and quickly evaluate the meta-aramid short fiber dyeability.

The present invention described above is not limited to the above-described embodiments, and various substitutions, modifications, and changes can be made without departing from the technical spirit of the present invention. It will be obvious to him.

Claims (9)

In the dyeing evaluation method of meta-aramid short fibers,
A refining step of immersing and refining the meta aramid short fibers in a refining solution which is an aqueous solution of 0.5 to 3.0% of soda ash;
A dyeing step of dyeing the refined meta-aramid short fibers in a salt bath of 20 to 40 g / L of acetophenone as a carrier and 0.5 to 20% of an aqueous basic dye of CI Basic;
A reduction step of reducing the dyed meta-aramid short fibers by immersing the short fibers in a reducing solution which is an aqueous solution of 0.5 to 1.5% of soda ash;
Water washing and drying step of washing the reduced meta-aramid short fibers with water and drying; And
And a dyeability evaluation step of evaluating the dyeability of the dried meta-aramid short fibers. The method of claim 1,
A dyeing evaluation method of meta-aramid short fibers, characterized in that the opening step of opening the meta-aramid short fibers before the refining step. The method of claim 1,
The refining process is a method for assessing the dyeability of meta-aramid short fibers, characterized in that the short fibers are immersed in the refining solution at 70 ~ 100 ℃ for 30 to 80 minutes. The method of claim 1,
The dyeing step is a method for evaluating the dyeability of meta-aramid short fibers, characterized in that the short fibers are immersed in a dye bath at 100 ~ 150 ℃ 30 to 100 minutes. The method of claim 1,
The dyeing evaluation method of the meta-aramid short fibers, characterized in that the addition of more than 0.3 ~ 0.7g / l alkyl ethoxylate-based leveling agent, 15-30g / l sodium nitrate for uniform dyeing in the dyeing process. The method of claim 1,
PH of the dye bath in the dyeing step is a dyeing evaluation method of the meta-aramid short fibers, characterized in that 2 to 5. The method of claim 1,
The reduction step is a method for evaluating the dyeability of meta-aramid short fibers, characterized in that the short fibers are immersed in the refining solution at 70 ~ 100 ℃ for 15 to 80 minutes to reduce. The method of claim 1,
The meta aramid short fibers are used for assessing the dyeability of meta aramid short fibers, characterized in that 3 to 10g. The method of claim 1,
The dyeability evaluation process is a method for assessing the dyeability of meta-aramid short fibers, characterized in that the color difference L value of 90 ~ 99, dyeing ratio of 90 ~ 99% of the standard cotton in the same dyeing and evaluation.

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