KR900003332B1 - The method of polyamide fiber - Google Patents

Abstract

A dyeable polyamide fiber is prepd. by adding 0.01-3.0 wt.% diamino alcohol of formula, H2N-(CH2)n-NH-R-OH (where n-1-10, R= alkylene of less than C5), w.r.t. produced polyamide during the polymerization; and spinning and stretching the obtd polyamide as a chip. Pref. the diamino alcohol cpd. is 2-(2-amino ethyl amino) ethanol or 2-(2-amino ethyl amino) isopropanol. The obtd. poly amide has good UV- durability, anti-pollution properties to absorption of Fe in water- treatment, washing-durability and frictiondurability

Description

Method for producing polyamide fiber with excellent dyeability

The present invention relates to a method for producing a polyamide fiber excellent in dyeing properties.

Polyamide, a thermoplastic copolymer, is widely used as a fiber because of its superior physical and chemical properties compared to other polymers. However, polyamide fibers have a low dyeing ability due to acid dyes and direct dyes, making it difficult to concentrate them with these dyes. This is because the dyeability of the polyamide depends on the number of amino groups at the terminal because the number of amino groups at the terminal is small in the polyamide. In order to improve the above drawbacks, a method of adding diamines (JP-A 44-19264), bis alkyrene triamines (British patent 1, 226, 944), etc., is known during polycondensation. Polyamides have a problem of deterioration due to ultraviolet rays and heat absorption during heat treatment, in particular iron adsorption in water, and deterioration in strength during high temperature treatment such as spinning, compared to pure polyamides. The addition method after the polycondensation of tertiary amino alcohols (JP-N 49-7080) and polyalkyrene imines (JP-N 46-25258) invented thereafter solved most of the above problems. As a problem, polyamide by the addition of tertiary amino alcohols has low dyeing fastness, and the polyalkyrene imine addition method is difficult to synthesize, and the obtained polyamide has a problem of poor leveling.

The present inventors have conducted a lot of research to solve the above problems simultaneously, and have come to invent a method for producing a polyamide having remarkably good dyeability compared to a pure polyamide without degrading the excellent properties of the pure polyamide. The present invention is a method for producing a highly dyed polyamide fiber characterized in that these additives are uniformly contained in the polyamide by adding 0.01-3.00% by weight of the diamino alcohols to the polyamide produced during the polyamide polymerization.

Diamino alcohols used for this invention are compounds which have the following general formula (I).

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H ₂ N— (CH ₂ ) _n —NH—R-0H... … … … … … … … … … … … … … … … … … … … (I)

Provided that n; Integer between 1-10, R; Alkyrene groups having 5 or less carbon atoms.

Examples of compounds of formula (I) include 2- (2-amino ethyl amino) ethanol, 2- (2-amino ethyl amino) isopropanol, 2- (3-amino propyl amino) ethanol, 2- (3-amino Propyl amino) isopropanol, 4- (2-amino ethyl amino) butanol, 3- (3-amino propyl amino) propanol and the like.

Diamino alcohols used in the present invention have a primary amino group, a secondary amino group, and a primary or secondary alcohol group as a functional group. The primary amino group of the diamino alcohol reacts with the carboxyl terminus of the polyamide to form an amide bond, changing the terminus to a terminal having a secondary amino group and an alcohol group. Secondary amino groups have higher stability by infrared rays and heat than those of primary amino groups, and have low dyeing ability to metals such as iron, and have similar dyeing ability to acid dyes and direct dyes. And alcoholic groups are stable functional groups and have considerable dyeing ability for acid dyes and direct dyes.

Therefore, when the diamino alcohol is used as an additive, deterioration due to infrared rays, adsorption of metals during the water treatment process, strength decrease during high temperature processes such as spinning, etc. can be significantly reduced, and sufficient dyeing performance can be improved. Moreover, homogeneity and fastness are also high by adding during polymerization to participate in the polycondensation reaction.

In the present invention, the above-mentioned diamino alcohols are added in an amount of 0.01-3.00% by weight with respect to the resulting polyamide during polyamide polycondensation. Particularly, when the amount of diamino alcohol is 0.05-2.0% by weight, a good effect is obtained. If the amount of diino alcohol added is 0.01% by weight or less, sufficient dyeing capacity cannot be imparted to the polyamide, and if it exceeds 3.00%, the strength of the polyamide is sharply lowered, which is not good.

The fulleramide obtained by the present invention is then melt spun and injection molded into various products. Compared to conventional polyamides, these products have excellent dyeing properties with good washing fastness and friction fastness while significantly reducing contamination due to premature degradation due to ultraviolet rays and absorption of iron during water treatment.

Example 1

2 kg of ε-caprolactam, 600 g of water, and a predetermined amount of 2- (2-amino ethyl amino) ethanol (see Table 1) were put into a 51 auto crave having a heating medium outside, and the air in the auto crave was replaced with nitrogen. Seal the autoclave and apply heat to reach internal pressure of 17.5kg / ㎠ and internal temperature of 260 ℃. After maintaining this temperature and pressure for 2 hours while discharging a small amount of steam, the pressure is gradually reduced to 60 minutes for 60 minutes, and then maintained for 90 minutes, and then discharged and cooled by applying pressure with nitrogen to make chips. The chip is rinsed, dried and melt-spun to obtain 260D / 18F undrawn yarn, followed by cold drawing at 3.7 times to obtain four 70D / 18F drawn yarn. Relative viscosity (? Rel) was measured in a conventional manner in 25 ℃ methacresol solution and the dyeing rate was measured by the following method. Acid dyes Coomassie Utra Sky SE (British ICI) 3% owf, acetic acid 1% owf, bath ratio 1: 40 owf After immersing the stretched yarn obtained in a salt bath and maintaining the dye at 90 ° C for 50 minutes, the solution balance and the initial stage The dye bath was measured with a colorimetric system to find the dye consumption.

Example 2

Other conditions were the same as in Example 1 except that a predetermined amount (see Table 1) of 2- (2-amino ethyl amino) isopropanol was used instead of 2- (2-amino ethyl amino) ethanol.

Comparative Example 1

0.25 weight% of acetic acid was used instead of 2- (2-ino ethyl amino) ethanol of the Example.

Comparative Example 2

0.50% by weight of hexamethylene diamine was used instead of 2- (2-amino ethyl amino) ethanol of the examples. Table 1 below shows the physical properties and dyeing properties of the chips and the drawn yarns obtained in the respective examples.

TABLE 1

Claims (2)

The polyamide is prepared by adding 0.01-3.0% by weight of diamino alcohols of the following general formula (I) to the resulting polyamide during the polymerization of polyamide. Method for producing amide fibers. bottom H ₂ N— (CH ₂ ) _n —NH—R—OH. … … … … … … … … … … … … … … … … … … … (I) Provided that n; An integer of 1-10, R; Alkyrene groups having 5 or less carbon atoms. The method for producing a polyamide fiber having excellent dyeability according to claim 1, wherein the compound of formula (I) is 2- (2-amino ethyl amino) ethanol or 2- (2-amino ethyl amino) iso propanol.