KR930008604B1 - Dyeing process and dyestuff formulation for carrying out the process - Google Patents

Abstract

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Description

[Name of invention]

High-temperature high-speed dyeing method of polyester fiber and polyester blend fiber using mixture of same color disperse dye

Detailed description of the invention

The present invention is characterized in that polyester fibers and polyester blend fibers are dyed using a mixture of two or more of the same color disperse dyes having a difference of each diffusion variable "D" of 2.4 or less and a disproportion variable "UL" of 5 or less. It relates to a novel method of high temperature high speed dyeing.

This method is suitable for dyeing raw materials, yarns, woven fabrics and knitted fabrics on dyeing machines known in dyeing methods such as pad dyeing machines, dyeing machines, jet dyeing machines, non-staining machines and continuous range dyeing machines.

Fast dyeing is known per se and is described, for example, in Federal Republic of Germany 3,241,727 (= British Patent Application No. 2,114,165).

The dye parameters mentioned above are actually similar to what is known and will be described in more detail later. The difference in diffusion variables is preferably less than 2.0.

The dye mixture is preferably used in the form of a composition obtained by treating the mixed press cake with a special dispersant mixture.

The dispersant mixture of a) a sulfur content of 4 to 6% by weight and an average molecular weight of 1500g ^-1 mol of lignin sulfonate (type I), b) a sulfur content of at least 6% by weight, an average molecular weight of 6,500g mol ^{- 1} of lignin sulfonate (type ⅱ), and c) a cycloaliphatic or an aromatic sulfonic acid and formaldehyde, and that the-composed of a salt condensation product (the ⅲ type), where the molecular weight of Sephacryl S-300 (SEPHACRYL S 300 The molecular weight distribution was recorded by refractive index analysis using a separation gel, and calibrated in 0.9% NaCl solution, and measured by aqueous gel permeation method measured in comparison with known dextran molecular weight.

Suitable dispersants I and II are commercially available products obtained by sulfite pulping wood.

Suitable dispersants of type III are in particular condensation products of aromatic sulfonic acids with formaldehyde [eg, (alkyl) naphthalene sulfonic acids, mixtures of naphthalene sulfonic acids and benzenesulfonic acids, sulfinated diphenyl ethers, sulfonated diphenyl thioethers , An alkali metal salt and an ammonium salt of sulfonated diphenylsulfone, and a formaldehyde condensation product of a mixture of cycloalkanon and an alkali metal bisulfite.

Such products, which are preferably used in the form of low-electrolyte, are described in US Patent No. 2,315,951, British Patent No. 715,919, German Patent Application No. 2,442,514, German Patent Application No. 2,542,090, Germany Federal Patent Application No. 2,856,222.

The disperse dyes present in the novel compositions can vary widely from a chemical point of view, provided they first meet the above requirements. Examples of these include sulfo-free dyes (eg, quinophthalone dyes, nitro dyes, methine dyes, naphthoquinoimine dyes, styryl dyes, azostyryl dyes, naphthos that are water-soluble only at room temperature). Perinone dyes and especially anthraquinone dyes, and azo dyes such as monoazo and disazo dyes).

The composition of the present invention comprises 15 to 50% of the primary dyes, 50 to 120% of the dispersant of type I and the dispersant mixture of type II and type III having a mixing ratio of 0.1 to 1.1: 1 to 0.1 with respect to the primary dyes used 30 To 120%.

In the present invention, "primary dye" means a pure raw dye, as obtained by drying from a presscake.

These compositions are obtained by mixing the dye presscake and then grinding to the desired particle size in a conventional grinding device and optionally by subsequent spray-drying.

Compared with each individually treated dye, the dyes dyed by the novel method of the present invention have improved remarkably in terms of heat transfer fastness and reserve in adjacent fibers (eg, cellulose and / or wool). .

Dyeing Example

Example 1a

100 parts of the textured polyester knitwear are dyed in a jet dyeing machine using a salt solution composed as follows: 0.5 part of the dye mixture prepared in Example 3b, 0.5 part of the dye mixture prepared in Example 4b, 1 part Warming aid (composed of 50 parts nonylphenol 10 ethylene oxide and 50 parts oleic acid 6 ethylene oxide), 1 part dispersant (sulfonated naphthalene-formaldehyde condensation product), 2 parts 60% strength acetic acid, 995 parts water.

The salt solution is heated rapidly to 80 ° C. and from 80 ° C. to 130 ° C. over 30 minutes. The temperature of 130 degreeC is hold | maintained for 20 minutes. After cooling, normal washing is performed and alkali reduction washing is performed.

As a result, a completely uniform, bright orange dye is obtained, which is excellent in wet and friction fastness even after application to subsequent heat-setting at 180 ° C. for 30 seconds.

Heat transfer dyeings are washed at 60 ° C. with adjacent multiple fibers in accordance with DIN 54017 to test heat dye fastnesses.

The criterion of measurement was the degree of contamination of nylon on a gray scale of grades 1-5. According to this test method, the dyeings were measured at levels 4-5.

Example 2a

100 parts of blended yarn of 50% polyester and 50% cotton are dyed in a cheese dyeing apparatus consisting of 1000 parts of a dye solution: 0.1 part Dye mixture prepared in Example 6b, 0.1 part Prepared in Example 5b Dye mixture, 0.8 part Dye mixture prepared in Example 8b, 995 parts water.

Further salt bath addition is as described in Example 1a).

The dyeing procedure is the same as in Example 1a), with the result that the polyester part was dyed in the dark blue color of the complete leveling, and the cotton fiber part was obtained completely uncontaminated. This dyeing is excellent in wet and friction fastness even after being subjected to subsequent heat setting at 180 ° C. for 30 seconds.

The contamination of nylon was measured by washing at 60 ° C. according to DIN 54017, which was measured as grades 4-5.

[Measurement of Diffusion Variable "D"]

A strip of polyethylene tetraphthalate film (Hostapha R 15; Hoechst AG) 4.5 cm wide by 15 cm thick was developed in boiling water without injecting air onto a 1.4 cm diameter VA stainless steel tube. The ends of the strip are attached parallel to the VA stainless steel tubes with thin VA stainless steel rods and elastic bands. The film wound tube is introduced into a HT beaker with 200 ml of a dye solution (0.5 g dye per liter) of pH 4.5 (controlled with acetic acid and Na acetate) and treated at 130 ° C. in a temperature controller for 5 1/2 hours. After the treatment time has elapsed, the tube with the film is simply washed with water, and the film is spread on the filter paper and air dried. The extinction coefficient of each layer (determined by a thin VA stainless steel rod) is measured optically and the diffusion parameter is calculated according to the method of Sekido et al. (Kogyo Kagaku Zasshi 68 (1965) 524). Diffusion variable D is in units of 10 ^-10 cm ² / sec.

[Measurement of Uneven Variable "UL"]

The cross-winding package is dyed on a 1974 type S 4566 Seprotec Laboratory dyeing machine, supplied with dyes corresponding to 1/10 standard chromaticity concentrations under the following conditions: liquid ratio 17: One ; Two liquid cycles per minute from the inside to the outside; Conical Package: 4 ° 20 ', 55 × 35 × 145mm from center; 750 g of dark 54 spun yarn; Double metric count 30; Outer diameter 160mm; Package density 365 g / l. 50 g of nonyl phenol containing 10 moles of ethylene oxide and 50 g of oleic acid containing 50 parts of sulfonated naphthalene / formaldehyde condensation product and 50 parts of sulfonated ditolyl ether / formaldehyde condensation product, 1 g / l, pH = 4.5 (controlled with acetic acid).

The temperature was raised from 80 ° C. to 2 ° C./min, heated to 130 ° C. and dyed at 130 ° C. for 10 minutes, followed by reduction washing in a conventional manner. Samples of the inner and outer layers of the package are taken. Dye is extracted from this sample using chlorobenzene. The concentrations C inside and C outside are measured optically. Disproportionate variables are as follows:

Processing Example

Example 1b

After mixing 259 g of the aqueous press cake of dye A described in Table I with 250 g of a dispersant of type I, correcting the pH to add a humectant, the mixture was bead-milled and the suspension was formed from type II and Dilution with a dispersant mixture of type III results in 30% of the primary dyes in the solid component and spray drying.

Example 2b

Instead of dye A of Example 1a, dye B is used as the same mixing ratio and mixed at the same mixing ratio.

Examples 3b to 9b show different mixing ratios, and the dyeings obtained by treating in the same manner as in Example 1a were excellent in flame retardancy and color fastness of cotton, and adsorbed so that vivid colors appeared. These mixtures are likewise suitable for the polyester / hair.

Table I (Dye Mixture)

Rf = residual moisture content

TABLE IIa (Dye Used)

TABLE IIb (Dye Used)

Claims (10)

Polyester fibers and poly, characterized in that they are dyed using a mixture of 2 to 10 same color disperse dyes with a difference of diffusion variable "D" of 2.4 to 0 and their disproportionate variable "UL" of 2 to 5. How to dye ester blend fibers at high temperature and high speed. The method according to claim 1, wherein the dyeing is carried out using a mixture of the following structural formulas (D) and (E) dyes.

The method according to claim 1, which is stained using a mixture of the following structural formulas (A), (B), (D) and (G) dyes.

The method according to claim 1, which is stained using a mixture of the following structural formulas (C), (B) and (G) dyes.

The method according to claim 1, which is stained using a mixture of the following structural formulas (F), (D) and (E) dyes.

The method according to claim 1, which is stained using a mixture of the following structural formulas (K), (L), (H) and (F) dyes.

The method according to claim 1, which is stained using a mixture of the following structural formulas (F), (L), (H), (K) and (C) dyes.

2. The dye according to claim 1, wherein the dye comprises (a) lignin sulfonate (type I) having a sulfur content of 4 to 6% by weight and an average molecular weight of 1500 g mol ^-1 , and (b) a sulfur content of 6 to 8.1%. A mixture of a dispersant comprising a lignin sulfonate (type II) having a weight percentage of 6500 g mol ⁻¹ and a (C) a low salt condensation product of a cycloaliphatic or aromatic sulfonic acid with formaldehyde (type III) [ Here, the molecular weight distribution is a method of correcting the molecular weight distribution by refractive index analysis method using SEPHACRYL S 300 separation gel and correcting in 0.9% NaCl solution. It is measured by the aqueous gel permeation method to be measured by comparison]. 10. A polyester fiber material dyed using the method of any one of claims 1-8. As a dispersant, (a) Lignin sulfonate (type I) having a sulfur content of 4 to 6% by weight, an average molecular weight of 1500 g mol ^-1 , (b) a sulfur content of 6% to 8.1% by weight, and an average molecular weight A mixture of this 6500 g mol ^-l lignin sulfonate (type II) and (c) a low salt condensation product (type III) of an alicyclic or aromatic sulfonic acid with formaldehyde [wherein the molecular weight distribution is cepacryl Molecular weight distribution was recorded by refractive index analysis using SEPHACRYL S 300 separation gel and calibrated in 0.9% NaCl solution, and measured by aqueous gel permeation method compared with known dextran molecular weight. Disperse dye composition containing;