JPH07207181A - Dye composition - Google Patents

Abstract

PURPOSE: To obtain a dye compsn. suitable for rapidly dyeing polyester fibers and polyester compounded fibers at high temp.

CONSTITUTION: A disperse dye compsn. contains a dispersant comprising a mixture of (a) a lignin sulfonate with a sulfur content of 4-6 wt.% and an average mol.wt. of 1,500 g mol^-1, (b) a lignin sulfonate with a sulfur content of at least 6 wt.% and an average mol.wt. of 6,500g mol^-1 and (c) a low salt condensation product of an alicyclic or aromatic sulfonic acid and formaldehyde and, herein, the mol. t. is measured by an aq. gel permeation method wherein a mol.wt. distribution is recorded by a refractometer using a Cephacryl S300 separating gel to be applied to a known dextran mol. wt. by a calibration curve in a 0.9% strength NaCl soln.

COPYRIGHT: (C)1995,JPO

Description

Detailed Description of the Invention

The invention uses a composition of at least two monochromatic disperse dyes such that the difference in diffusion parameter "D" is less than 2.4 and the disproportionate dyeing parameter "UL" is less than 5. The present invention relates to a high-temperature rapid dyeing method for polyester fibers and polyester-blended fibers, which comprises performing dyeing.

The process is, for example, pad dyeing--machines, yarns--
Disaggregated materials on known dyeing machines for individual process steps such as dyeing machines, jets, beams and continuous areas,
Suitable for dyeing yarns, fabrics and knits.

Rapid dyeing processes are known per se and, for example, German publication 3,241,727 (= UK patent 2,
114,165).

The dye parameters mentioned above are likewise known per se, and more will be explained in more detail below. The difference in diffusion parameters is preferably less than 2.0.

The dye compositions are preferably used in the form of compositions obtained by treating the combined presscakes with a particular dispersant composition.

The dispersant composition comprises a) a sulfur content of 4-6% by weight and 1,500 gmol.
A lignin sulfonate having an average molecular weight of ^-1 (type I), b) a sulfur content of at least 6% by weight and 6,500
a lignin sulfonate having an average molecular weight of g mol ^-1 (type II), c) a low-salt condensation product of alicyclic or aromatic sulfonic acids with formaldehyde (type III), wherein Molecular weights were recorded on a refractometer using a SEPHACRYL S 300 preparative gel and the molecular weight distribution was determined by calibration with a calibration curve in 0.9% strength NaCl solution to a known dextran molecular weight. It is measured by the method.

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

Suitable dispersants of type III are, in particular, condensation products of aromatic sulphonic acids with formaldehyde, for example (alkyl) naphthalene sulphonic acids, mixtures of naphthalene sulphonic acids and benzene sulphonic acids, sulfinated diphenyl ethers, Potassium metal and ammonium salts of sulfonated diphenyl thioethers, sulfonated diphenyl sulfones and formaldehyde condensation products of mixtures of cycloalkanones and alkali metal bisulfites.

Such products, which are preferably used in the low-electrolyte form, are reiterated in the literature; eg US Pat. No. 2,315,951, British Patent Publication 71.
5,919, German Patent Publication 2,442,514, German Patent Publication 2,542,090, German Patent Publication 2,8
56,222.

The disperse dyes present in the novel compositions can be diverse from a chemical point of view, so long as they meet the conditions mentioned at the outset. They are, for example, sulfo-free dyes which are slightly soluble at room temperature, such as quinophthalone dyes, nitro dyes, methine dyes, naphthoquinimine dyes, styryl dyes, azostyryl dyes,
Naphthoperinone dyes and especially anthraquinone and azo dyes, such as monoazo and disazo dyes.

The composition has a raw color of 15 to 50%, a dispersant of type I of 50 to 120% with respect to the raw dyestuff used and a mixing ratio of 30 to 120% of 0.1 to 1.1: 1 to
It contains a mixture of Type II and Type III dispersants which vary to 0.1.

"Green color" is to be understood as meaning, for the purposes of the present invention, a pure, untreated dye, such as that obtained by drying from presscakes.

These compositions are obtained by mixing dye presscakes, followed by grinding in a conventional grinding machine to the desired particle size and, if desired, then spray drying.

Compared to individually treated dyestuffs, the dyeing in the novel process gives surprisingly improved thermophoretic fastness on adjacent fibers, cellulose and / or wool.

[0015]

Dyeing Examples Example 1a 100 parts of woven polyester knitwear in a jet dyeing machine, 0.5 parts of the dye mixture from Example 3b, 0.5 parts of the dye mixture from Example 4b. 1 part nonionic leveling aid (consisting of 50 parts nonylphenol 10 ethylene oxide and 50 parts oleic acid 6 ethylene oxide), 1 part dispersant (sulfonated naphthalene-formaldehyde condensation product), It was treated with a dyeing solution consisting of 2 parts of 60% strength acetic acid and 995 parts of water.

The liquid is rapidly heated to 80 ° C. and
To 130 ° C. for 30 minutes. A temperature of 130 ° C was maintained for 20 minutes. Cooled, then generally rinsed and alkaline reduction clarified.

The result obtained is a completely uniform, bright orange dyeing. This dyed product is dyed at 180 ° C.
It had excellent wet and rub fastness even when heat set at 30 seconds.

Thermophoresis fastness was tested on heat-set dyeings by washing at 60 ° C. with adjoining blended fibers according to DIN 54017.

The criterion for evaluation was the coloring of the nylon measured against a gray scale of 1-5. Using this test method, the above staining was rated 4-5.

Example 2a 100 parts of 50% polyester and 50% cotton blend yarn in a cheese dyeing machine, 0.1 part of the dye mixture from Example 6b, 0.1 part of the dye from Example 5b. blend,
Treatment was carried out with 1,000 parts of a solution consisting of 0.8 part of the dye mixture from Example 8b, 995 parts of water.

The other dyebath additives were as described in Example 1).

The dyeing process was as described in 1). The result obtained on the polyester part was a deep, completely uniform deep blue dyeing. The cotton fibers remained completely unpigmented. This dyeing is then
It had excellent wet and rub fastness even when heat set at 0 ° C. for 30 seconds.

DIN as measured by coloring nylon
A 60 ° C. wash according to 54017 was rated 4-5.

Diffusion parameter “D” measured thickness 15 μm, width 4.5 cm and length 65 c.
m polyethylene terephthalate film (Hosta
pha R15, Hoechst AG) was spread in boiling water on a VA stainless steel tube with a diameter of 1.4 cm with exclusion of air. One end of the piece was connected to a VA stainless steel tube with a thin VA stainless steel and elastic band. Pipe the unrolled film in a HT beaker to a pH of 200 ml.
A dye solution of 4.5 (adjusted with acetic acid and Na acetate) (0.5 g of dye per liter) was added and treated in a thermostat at 130 ° C. for 5 and a half hours. At the completion of the treatment time, the tube with the film was briefly rinsed with water, the film was spread on filter paper and dried in air. The extinction of the individual layers (marked by thin VA stainless steel rods) was measured spectrophotometrically, and Sekid et al., Journal of Industrial Chemistry 68 (1965), 524.
It was used to calculate the diffusion coefficient by the method of. The diffusion parameter D is the diffusion coefficient in the unit of 10 ⁻¹⁰ cm ² / sec.

Determination of the Disproportionate Dyeing Parameter "UL" A dye which constitutes a standard color depth of 1/10 under the following conditions in a 1974 S4566 Seprotec laboratory dyeing machine in a cross-wrap package: Was supplied and stained.

Liquid ratio of 17: 1, liquid circulation from inside to outside twice per minute.

Conical packaging; 4 ° 20 'center, 55 × 33
X 145 mm; 750 g Dacron 54 spun yarn, double metric rating 3
0: maximum outer diameter 160 mm; packing density 365 g / liter. 1 g / l of 50 parts nonylphenol and 1
3. Leveling agent consisting of 0 mol of ethylene oxide, 50 parts of oleic acid and 50 parts of sulfonated naphthalene / formaldehyde condensation product and sulfonated ditolyl ether / formaldehyde condensation product, respectively; pH = 4.
5, adjusted with acetic acid.

Temperature process: 80 ° C to 2 ° C per minute to 130 ° C
Heated and dyed at 130 ° C. for 10 minutes. afterwards,
It was reduced and clarified normally. Samples of the outer and inner layers of the package were taken. The dye was extracted from the sample with chlorobenzene. The concentration inside C and outside C was measured with a spectrometer. The uneven dyeing parameter is

[0029]

【number】

It is

Treatment Examples Example 1b 259 g of an aqueous presscake of the dye A listed in Table I are mixed with 250 g of the dispersion of type I and the mixture is--
After pH correction and addition of humectant--bead milled and the dispersion was used with a type II / III dispersant mixture containing 30% of the raw color in the solid content and spray dried. In such a way that a
Diluted.

Example 2b Instead of dye A in example 1, dye B could also be used in the same mixing ratio.

Examples 3 to 9 describe combinations treated according to Example 1 and characterized by very good to good cotton retention and fastness and shade exhaustion. These mixtures were likewise suitable for polyester / wool.

[0034]

[Table 1]

[0035]

[Table 2]

[0036]

[Table 3]

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Fredgarh Hoffmann Day 4018 Germany Federal Republic of Germany 4018 Langenfert Brunz Atzka Schyutraße 13 (72) Inventor Erhard Schyufuenhauer Day 5090 Lefelkusen 1 Germany・ Friedrich-Bayer-Schütlerse 13 (72) Inventor, Wolfgang Heebler, Federal Republic of Germany Day-5068 Odenter Le Michael Hähe 23

Claims (1)

[Claims] 1. A lignin sulfonate (type I) having a sulfur content of 4-6% by weight and an average molecular weight of 1,500 gmol ^-1 , b) a sulfur content of at least 6% by weight and 6, 500
a mixture of a lignin sulfonate having an average molecular weight of g mol ^-1 (type II), c) a cycloaliphatic or aromatic sulfonic acid and a low-salt condensation product of formaldehyde (type III) as a dispersant The molecular weight distribution here is the molecular weight distribution SEPHACRYL S
Record in the refractometer using a 300 preparative gel and 0.
A disperse dye composition measured by an aqueous gel permeation method in which a known dextran molecular weight is applied by a calibration curve in a 9% strength NaCl solution.