DE2657216B1 - 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 DT-AS 22 13 241 that cellulose fibers and their mixtures with synthetic fibers Fibers with water-insoluble azo dyes produced on the fiber in one bath using the exhaust method let it be dyed if an aqueous liquor is allowed to act on the textile material at about room temperature, In addition to alkali sodium nitrite and an anionic dispersing system, the solution or dispersion 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 contains, and then after pulling the coupling component through Addition of acid or acid salts to the dyebath at room temperature, the diazotization of the amine and the Induces dye formation by coupling on the fiber

However, such dyeing is still time consuming or special apparatus is required which z. B. by applying pressure differences in the case of the use of pressure equipment a shortening of the Allow dyeing time. The necessary pressure differences are generated at elevated temperatures

worked

The object of the present invention is now to provide a rapid dyeing exhaust process for the development of azo pigments on cellulose fibers

5 or mixtures of cellulose fibers with synthetic fibers, which allows without the Application of atmospheric pressure at normal temperature (20 ° to 40 ° C) on usual Apparatus to work and being a time gain

ίο compared to those known from the prior art Staining methods in this field can be achieved.

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. Such a solution 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 a higher static pressure - the primer of the textile material with this liquor at a bath circulation or a material circulation of at least five times per minute, and at temperatures from 10 ° to 40 ⁰ C, preferably 15 ° to 25 ° C, takes place in the course of 10 to 20 minutes, then with the help of organic acids, the pH of the dyebath quickly changed to acidic conditions and then heated the same to temperatures of 30 ° to 50 ⁰ 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 help of an im

The anionic dispersants used in this dyebath are not coarse despite the single-bath mode of operation Dye pigments are deposited on the fiber surface, so that the aftertreatment is also essential is 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 consists in adding the necessary naphthol and the necessary base to the dyebath, the anionic dispersant, sodium hydroxide solution, optionally 10 to 30 g / l salt and the sodium nitrite required for later diazotization, and the textile material at 10 to 40 ⁰ C, preferably at 15 to 25 ° C, is treated with this primer bath for 10 to 20 minutes. The liquor is then acidified quickly with organic acid, whereby the diazotization and coupling of the azo dye generally takes place at 30 ° to 50 ° C. This is followed by the aftertreatment customary for azo developing dyes.

For the production of the colorations according to the claimed process, those come from the ice color technique well-known coupling components into consideration, according to the method only those with substantive or highly substantive character can be used in relation to the fiber material. Here it is a matter of compounds that couple to a hydroxyl group in the vicinity and none of them are soluble Have making groups, in particular arylamides of aromatic or heterocyclic o-hydroxycarboxylic acids or from acyl acetic acids and other aromatic or heterocyclic hydroxy compounds and compounds containing an enolizable or enolized ketomethylene group which are mutually exclusive located in a heterocyclic ring Such substances are, for example, arylamides of

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-hydroxydiphenylene 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 method according to the invention can be based on the known cellulosic fibers and mixtures Synthetic fibers, e.g. B. polyester fibers, and cellulose fibers can be used. With 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 that outside the fiber Azo pigment formed 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 ο Such a cooling of the material to be dyed can be achieved by applying a negative pressure.

example 1

Cotton bobbin, in a Kreuzspulenfärbeapparat at a bath circulation of 6 times per minute, for 15 minutes at 30 ⁰ C with an aqueous liquor (liquor ratio 1:10), which

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

5 g / l of a 50% amine dispersion from Azoic

Diazo Component 5 - CI No. 37 125, dispersed with polyethylene glycol from the mol-wt. 600 and ethylene glycol,
3 g / l of an anionic protective colloid based on an oleic acid protein hydrolyzate

Condensation product,
6cm ³ / l 32.5% sodium hydroxide solution (= total amount, including the amount required to release the above coupling component),

3 g / l sodium nitrite and
20 g / l sodium chloride

After this priming phase of the winding body, this liquor is used for the purpose of lowering the pH value

^{10 cm 3} / l lactic acid 80% and
10 cm ³ / l formic acid 85%

and continues the treatment of the goods for 10 minutes at 40 to 45 ° C under the set acidic Conditions continue during which the diazotization of the amine and the development of the dye takes place. The aftertreatment of the textile material dyed in this way shows

so now the following operations:

5 minutes rinsing of the dye with water at 40 ° C,
10 minutes of grinding at 60 ⁰ 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;

5 minutes rinse 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

1 g / l of a high molecular 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 dyeing of a cotton fabric is done using a jet dyeing machine "System Thies" carried out at 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 / 1 denatured ethanol, is added to a mixture of 2.2 cm ³ / l of water at 70 ⁰ C and 1.1 cm ³ / l sodium hydroxide solution 32,5 ° / oig added and brings this approach under Stir 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 / l sodium hydroxide solution 32.5% (= total amount, including the amount used to release the coupling component), 10 g / l sodium chloride and 2 g / l sodium nitrite.

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

8.5 cm ³ / l 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 for 5 minutes with warm water 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;

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 / 1 Azoic Diazo Component 32 - C.I. No. 37 090

together with 7.2 cm ³ / l denatured ethanol made into a paste, and this paste is 1.1 cm ³ / l sodium hydroxide solution 32,5 ° / oig added After diluting with 4,4cm ³ / l water at 40 ⁰ C, the mixture is brought into solution with stirring. The solution obtained in this way is then poured into an aqueous bath template with the following composition:

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

6cm ³ / l sodium hydroxide solution 32.5% (= total amount, including the amount used to release 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

10cm ³ / l 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 containing 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 rinse with warm water for 5 minutes and

Soaped at the boil for 10 minutes with an aqueous bath, so for 10 minutes at 95 ° C. with an aqueous liquor with the addition of with the addition of

1 g / l oleylmethyltaurine (Na 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.

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. A method 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 by the exhaustion method using an aqueous liquor which, in addition to alkali, sodium nitrite and an anionic dispersing system, still has the solution or dispersion at least a 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, characterized in that - without the liquor and goods being exposed to an increased static pressure - the primer of the textile material with makes this liquor with a bath circulation or a material circulation of at least five times per minute and minutes, then with the help of organic acids, the pH of the dyebath is quickly converted to acidic conditions and then heated Lben dye formation causes to temperatures of 30 ° to 50 ⁰ C on the fabric by diazotizing and coupling in such a way that the total dyeing 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.