DE2657216C2 - Rapid dyeing process with insoluble azo dyes produced from the components on the fiber for cellulose fibers and their mixtures with synthetic fibers - Google Patents

Description

The two-bath dyeing of cellulose fibers by the exhaust process with dye components that are suitable for the formation of insoluble azo pigments on the fiber, according to the principle - coupling component in the primer bath, diazo component in the developer bath - has been known for a long time.

It is also known from DE-AS 22 13 241 that cellulose fibers and their mixtures with synthetic fibers with water-insoluble azo dyes produced on the fiber can be dyed in a single bath by the exhaust method if an aqueous liquor is allowed to act on the textile material at about room temperature, ^r ><> which, in addition to alkali sodium nitrite and an anionic dispersing system, also contains the solution or dispersion of at least one component capable of azo coupling and at least one undiazotized primary aromatic amine in a medium based on an M water-miscible organic solvent or solubilizer, and then after The coupling component is absorbed by adding acid or acidic salts to the dyebath at room temperature, which causes the amine to diazotize and w) dye formation by coupling on the fiber.

However, such dyeing is still time consuming or special equipment is required which, for. B. allow a shortening of the dyeing time by applying pressure differences in the case of M the use of pressure equipment. To generate the necessary pressure differences, elevated temperatures

The object of the present invention bes.leht is now to design a Schriellfärbe exhaust process for the development of azo pigments on cellulose fibers or mixtures of cellulose fibers with synthetic fibers, which allows without the use of atmospheric pressure at normal temperature (20 ° to 40 ° C) ⁰ C) to work on conventional apparatus and it is possible to save time compared to the dyeing methods known from the prior art in this field of work.

This task is - contrary to the expectations, experiences and ideas of a specialist - according to the invention by priming the goods with aromatic amine, nitrite and coupling component with the highest possible bath circulation and / or material movement, as well as subsequent single-bath diazotization and forcing the coupling released by increasing the bath temperature up to 50 ° C. One such The method advantageously does not require any pressure equipment.

The present invention relates to a process for the shortened, single-bath dyeing of textile materials, preferably in the form of wound packages, made of cellulose fibers or mixtures containing those with water-insoluble azo dyes produced on the fiber by the exhaustion method using an aqueous liquor which, in addition to alkali , Sodium nitrite and an anionic dispersing system or the solution or dispersion of at least one component capable of azo coupling and at least one undiazotized primary aromatic amine in a medium based on a water-miscible organic solvent or solubilizer, which is characterized in that - without liquor and goods are exposed to increased static pressure - the priming of the textile goods with this liquor with a bath circulation or a material circulation of at least five times per minute and at temperatures of 10 ° to 40 ° C, preferably 15 ° to 25 ° C ₁ makes in the course of 10 to 20 minutes, then with the help of organic acids, the pH value of the dyebath quickly changed to acidic conditions and then heating the same to temperatures of 30 ° to 50 ° C, the dye formation on the goods by diazotization and coupling in the Manner ensures that the total staining time does not exceed 30 minutes. With the aid of an anionic dispersant used in the dyebath, no coarse dye pigments are deposited on the fiber surface despite the single-bath procedure, so that the aftertreatment is also considerably simplified and shortened.

The process of the present invention provides a rapid dyeing method for azo developing naphthol-based dyes as it is considered absolutely impossible for this dyeing technique by the experienced practitioner became. The advantages of this new process lie in the simple, single-bath mode of operation through which Due to the product selection, the usual calculations of alkali binding capacity etc. not more are required. The considerable time savings and, last but not least, the good reproducibility of the Coloring as well as the fastness properties mean for the former ice color technology again a process-technical one Competitive to other dyeing processes for cellulose fibers. In this way, the

simple and inexpensive products of the well-known azo dye components also in the modern Rapid dyeing can be used advantageously in terms of process technology.

The principle of the present procedure is that the required naphthol and the required base the dyebath, the anionic dispersant, sodium hydroxide solution, optionally 10 to 30 g / l salt and the sodium nitrite required for later diazotization is added and that Textiles at 10 to 40 ° C, preferably at 15 to 25 ° C, treated with this primer bath for 10 to 20 minutes. Then the floite with organic acid made acidic quickly, whereby the diazotization and coupling of the azo dye in the generally takes place at 30 to 50 ° C. This is followed by an aftertreatment that is customary for azo developing dyes.

For the production of the colorations avenge the claimed The coupling components, which are well known from ice color technology, come from this process into consideration, whereby according to the procedure only those with a substantive or highly substantive character the fiber material are used. These are connections that are in neighboring positions couple to a hydroxyl group and have no solubilizing groups, especially arylamides of aromatic or heterocyclic o-hydroxycarboxylic acids or of acyl acetic acids and others aromatic or heterocyclic hydroxy compounds and compounds which have an enolizable or contain enolized ketomethylene group, which located in a heterocyclic ring. Such substances are, for example, arylamides

2,3-hydroxynaphthoic acid, the
2-hydroxyanthracene-3-carboxylic acid, the
4-hydroxydiphenyl-3-carboxylic acid, the
2-hydroxycarbazole-3 · carboxylic acid, the
3-hydroxydiphenyloxide-2-carboxylic acid, the
3-hydroxydiphenyl sulfide-2-carboxylic acid, the
Acetoacetic acid or benzoylacetic acid.

Furthermore, inter alia Hydroxybenzenes, polyhydroxybenzenes, Hydroxynaphthalenes and pyrazolones have proven to be suitable, if appropriate by nonionic substances Radicals are substituted.

According to the process, all primary aromatic amines can be used for the development of the azo dyes are used, the water-insoluble mono-, dis- or polyazo dyes, including aromatic diamines. The amines suitable here, to which also Aminoazo dyes count, have no ionic substituents and are diazo components from the Ice color technique known.

The inventive method can be based on the known cellulosic fibers and mixtures Synthetic fibers, e.g. B. polyester fibers, and cellulose fibers can be used. Pei the cellulose fibers in this context it is native fibers such as flax, hemp, linen and cotton, or around regenerated fibers such as viscose, rayon and modal fibers.

As an anionic dispersing system for the dye-forming Components and the azo pigment formed outside the fiber before and after the addition of acid are z. B. Auxiliaries based on 2,2'-dinaphthylmethane-6,6'-disulfonic acid Sodium or lignin sulfonate, optionally mixed with oleylmethyltaurine, used

Organic acids that can be used include Monochloroacetic acid. Lactic acid, formic acid or acetic acid can be used.

To speed up the priming, the material is well pre-wetted, removing the air Pre-steaming of the textile material can also take place within the wound body. A possibly required The material to be dyed can be cooled down by applying a negative pressure.

example 1

Cotton bobbins «./ earth in a cheesecloth dyeing machine, with a bath circulation of 6 times per minute, for 15 minutes at 30 ° C with an aqueous one Liquor (liquor ratio 1:10) treated which

3 g / l of the dissolved coupling component Azoic Coupling Component 8 - C. I. No. 37 525,

y, 5 g /! a 50% amine dispersion from Azoic

Diazo Component 5 - C.I. No. 37 125, dispersed with polyethylene glycol from Mole weight 600 and ethylene glycol,

3 g / l of an anion-active protective colloid based on an oleic acid protein hydrolyzate

Condensation product,

6 cmVI sodium hydroxide solution 32.5% (= total amount, including the men- tion required to release the above coupling component

! ■> ge).

3 g / 1 sodium nitrate and
20 g / l sodium chloride

contains. After this priming phase of the winding body 4 (i This liquor is used to lower the pH

10 cmVl lactic acid 80% and
10cmVl formic acid 85%! g

4> and continues treatment of the goods for 10 minutes at 40 to 45 ° C under the set acidic conditions, during which the diazotization of the Amine as well as the development of the dye takes place. The aftertreatment of the textile material dyed in this way shows

w now the following operations:

5 minutes rinsing of the dyeing with water at 40 ⁰ C,
10 minutes grinding at 60 ° C with an aqueous bath with the addition of

1 g / l of the reaction product of 1 mole of nonyl

phenol with 10 moles of ethylene oxide,
1 g / l soda calc. and
1 g / l of a high molecular weight polyphosphate;

bo 5 minutes rinsing with water at 60 ° C,

10 minutes of boiling soaps with an aqueous bath with the addition of

1 g / l oleylmethyl laurine (sodium salt)
1 g / l soda calc. and
^b> lg / l of a high molecular weight phosphate;

Rinse with warm water for 5 minutes as well
Rinse with cold water for 5 minutes.

A uniform red coloration of the wound body with good fastness properties is obtained.

Example 2

The coloring of a cotton fabric is under Use of a jet dyeing machine »System Thies« with a liquor ratio of 1:10. the Material speed is 5 revolutions per minute. For the production of the dye liquor are

2.2 g / l of the coupling component Azoic Coupling Component 32 - C. I. No. 37 580 and

2.9 g / l of the amine Azoic Diazo Component 3 - C.I. No. 37 010

slurried in 5.7 cm / i denatured ethanol, is added to a mixture of 2,2 CMVi water of 70 ⁰ C and 1.1 cm ³ / l sodium hydroxide solution 32,5% ig added and this approach brings with stirring in solution. This solution is then placed in a prepared aqueous bath, which contains the following auxiliaries and chemicals:

2 g / l of the condensation product of 2,2'-dinaphthylmethane-6,6'-disulfonic acid Sodium with m-cresol,

6 cm ³ /! 32.5% sodium hydroxide solution (= total amount, including the amount used to dissolve the coupling component), 10 g / l sodium chloride and

2 g / l sodium nitrite.

The textile material is primed for 20 minutes at 30 ° C with the liquor prepared in this way. Then you pass over the overflow

8.5 cmVI monochloroacetic acid

into the liquor cycle, whereupon from 30 ° to 45 ° C increasing temperature in the course of 10 minutes, the amine is diazotized and the dye is developed.

The goods dyed in this way are used for post-treatment

Rinsed with warm wawer for 5 minutes and
Soaped for 10 minutes at 60 ⁰ C with an aqueous bath with the addition of

1 g / l soda calc. and

1 g / l of a high molecular weight phosphate;

Rinsed with warm water for 5 minutes and
Soaped at the boil for 10 minutes with an aqueous bath with the addition of

1 g / l oleylmethyltaurine (sodium salt)

1 g / l soda calc. as

1 g / l of a high molecular weight phosphate;

Rinsed warm and cold with water for 5 minutes.

A uniform red dyeing of the cotton fabric with good fastness properties is obtained.

Example 3

The dyeing of terry toweling is done on a dyeing machine for strands of goods with bath circulation made a liquor ratio of 1:20. The bath is circulated 5 times per minute.

The fleet to be used is assessed as follows:

2.2 g / l Azoic Coupling Component 28 - C. I. No.

37 541 and
2.7 g / l Azoic Diazo Component 32 - CI No.

37 090

are made into a paste together with 7.2 cmVI denatured ethanol, and this paste becomes 1.1 cmVI sodium hydroxide solution 32.5% added. After dilution with 4.4 cmVI water at 40 ° C, the mixture is stirred in Solution brought. The solution obtained in this way is then poured into an aqueous bath template with the following composition given:

2 g / l of the condensation product of 2,2'-dinaphthyl-methane-6,6'-disulfonic acid Sodium with m-cresol,

6cm ³ / l 32.5% sodium hydroxide solution (= total amount, including the amount used to loosen the coupling component),
20 g / l sodium chloride and

2 g / l sodium nitrite.

With the dye liquor produced in the manner described, the goods are primed for 20 minutes at 30 ^° C. and then placed in this bath

10 cmVI acetic acid 60%

and diazotizes the amine and develops the dye in the course of 15 minutes at a temperature rising ^{to 45 ° C.}

The following operations are carried out to complete the dyed goods:

5 minutes rinse with cold water and
10 minutes of soaps at 60 ^° C. with an aqueous bath

1 g / l of the reaction product of 1 mole of nonyl

phenol with 10 moles of ethylene oxide,
1 g / l soda calc. and
1 g / l of a high molecular weight phosphate;

Rinse with warm water for 5 minutes and

Soap for 10 minutes at 95 ° C with an aqueous liquor with the addition of

1 g / l oleylmethyltaurine (sodium salt),

1 g / l soda calc. and

1 g / l of a high molecular weight phosphate;

Rinse with warm and cold water for 5 minutes.

This gives terry toweling which is dyed evenly red and has good fastness properties.

Claims (3)

Patent claims: 1. Process for the shortened one-bath dyeing of textile materials made of cellulose fibers or of ■> Mixtures containing such with water-insoluble azo dyes produced on the fiber the extraction method using an aqueous liquor, which in addition to alkali, sodium nitrite and an anionic dispersing system nor the solution or dispersion of at least one for Azo coupling capable component and at least one undiazotized primary aromatic Amine in a medium based on a water-miscible organic solvent or solubilizer contains, characterized in that - without the liquor and goods being exposed to an increased static pressure - The priming of the textile material with this liquor during a bath circulation or a material circulation at least five times per minute and minutes, then with the help of organic acids the The pH of the dyebath is quickly changed to acidic conditions and then heated same to temperatures of 30 ° to 50 ° C the 2ί Dye formation on the goods by diazotization and coupling in such a way that the Total staining time does not exceed 30 minutes. 2. The method according to claim 1, characterized in that the priming temperature 15 ° to 25 ° C. 3. The method according to claims 1 and 2, characterized in that textile materials in the form of Windings are colored.