DE3518149A1 - Two-phase steaming process for fixing prints containing reactive dyestuffs to keratin fibres - Google Patents

Abstract

The fixation of reactive dyestuffs to keratin fibres and blends thereof with cellulose fibres by steaming does not always lead, in particular in the presence of large patches of fabric, to acceptable dyeing results on account of the frosting and of the tippy dyeing caused by "drying-out" of the steamer. The existing defects are removed by means of the use of a two-phase steaming process, previously unknown in the case of keratin fibres, which provides for minimum-liquor application systems for the application of the fixing alkali applied to the preprint, together with the fixation of the dyestuffs in a festoon steamer.

Description

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HOECHSTAKTIENGESELLSCKA-PT-- HCS- 85 /? e3-6 Dr.CZ/sch

Two-phase steaming process for fixing prints with reactive dyes on keratin fibers

The present invention relates to a method for continuous Fixing of prints with reactive dyes on textile webs made of keratin fibers or theirs Mixtures with cellulose fibers using a two-phase steaming technique, the dissolved alkaline fixing agent in the form of minimal amounts of liquor on the unfixed, previously printed with the reactive dyes without the addition of alkali and hygroscopic agents and optionally dried Fiber material is applied.

The fixation of prints with reactive dyes on textile Sheet-like structures made of cellulose fibers according to the two-stage procedure with the inclusion of vapors carried out in practice for many years. For textiles made from keratin fibers, the application of a Such a fixation method, however, is not yet recommended because the special ones previously used for this purpose Two-phase dampers allow heat to be applied for only short steaming times of 5 to 30 seconds.

However, keratin fibers require a high moisture content in the damper and a long time in the fixing operation Steaming time to ensure a sufficient response between the Ensure dye and nitrogenous fiber. About the high heat of absorption of wool in the Damper is reported in particular in "Textile Research Journal", Volume 53 (1983), pages 125 to 141. One sets In the course of the conventional dye fixation on wool, the printing pastes therefore have high amounts of hygroscopic Substances - mainly urea and alkali - are added and the textile material is steamed for heat treatment with saturated steam 8 to 15 minutes in a hanging loop damper. In the case of dyeing small batches of goods, this works

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Known processes problem-free, but with larger loads the moisture content in the steamer drops continuously off, i.e. the steamer "dries out", which results in a gray haze and "sharp colorations" on the dyed wool.

The above-mentioned difficulties naturally also apply to mixtures of keratin and keratin for the same reason Cellulose fibers. A further complicating factor in the case of the latter is that reactive dyes are used for fixing on cellulose fibers require a relatively high amount of alkali, which in turn reduces the shelf life of the printing pastes deteriorated and, on the other hand, reduced the tear strength of the keratin fibers. At the moment, reactive dyes are used Fixed on mixed articles made of keratin and cellulose fibers, mainly using the two-phase short steaming process. In order to ensure the lowest possible reduction in tear strength with such a procedure, works In this case, reduced amounts of the alkaline fixing agent are added to the padding liquor and this is used a reduction in the color yield on both fiber components of the mixed materials.

Knowing the shortcomings of the relevant Processes known from the literature for fixing reactive dyes on keratin fibers were the task for the present invention now in accordance with the conventional methods in this field of work to modify the needs of the practice. In particular JO should find ways and means that allow to keep the moisture content of the wool constant during the steaming process and thereby the so-called "drying out" of the damper as well as the development of gray haze and sharp colors. For Mixtures of keratin and cellulose fibers should develop a process for printing with reactive dyes

which also ensures a good shelf life of the printing pastes, low fiber damage and optimal color matching on the various components of the Paser mixed materials.
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It has now surprisingly been found that commercially available reactive dyes can also be used in larger quantities of Keratin fibers or mixtures of keratin and cellulose fibers can be properly fixed by steaming, if you can the printing pastes with the reactive dyes without hygroscopics and alkali and then printed on to the first hand and optionally intermediate-dried goods, an alkali and optionally electrolyte-containing fixer solution applied in the attack by means of a minimal application device, and then for the purpose of dye fixation instead of a two-phase system based on the conventional construction principle, which is only used for brief steam treatment is designed, which is widely used in textile printing for the single-phase mode of operation begins.

The object set according to the invention is thus achieved solved that one as the fixing liquor aqueous solutions of sodium acetate trihydrate, optionally mixed with other alkalis and electrolytes, as well as the impregnation process to cover the pre-pressure with this Fixing liquor either as such or in the foamed state by means of a lower uniform application Application measure causing the amount of liquid (minimum application) undertakes, and that the subsequent Hitsefixierung the print on the treated textile material by long-term steaming in a hanging loop damper with Brings about saturated steam.

The principle of the present invention is based on discovery as well as the practice-oriented implementation of special guidelines for optimal process conditions that

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against the "previous knowledge and experience of the operational Concerns a transfer of the advantages of the two-stage fixing process for reactive dyes from the Cellulose permitted on keratin fibers. At the same time it was recognized that the problem of high heat of absorption of wool can be overcome by a two-phase process, and that one continues through the targeted use of a Two-phase steaming process previously unknown for keratin fibers based on the use of minimal application systems for the application of the fixing liquids or foams on the alkali-free preprint with the reactive dyes in combination with the subsequent dye fixation in a hanging loop damper is, the difficulties outlined above in the course of fixing prints with reactive dyes Get a grip on keratin fibers.

The composition of the fixing liquor is naturally whole in the claimed two-phase long steaming process different from the relevant recipe in the case of conventional two-phase short steaming processes. As an alkali for the fixation of reactive dyes on keratin fibers is, according to the invention, sodium acetate trihydrate, technically in one Concentration of 100 to 200 g per liter of water used.

In the case of the single-phase steaming process, on the other hand, in general the much more expensive sodium acetate anhydrous, chemically pure used. In the case of mixtures of keratin fibers cellulose fibers add 20 to 80 g of soda, pottache or caustic soda to the fixative solution Liters of liquor added. If necessary, 50 to 200 g / l table salt or Glauber's salt is used as the electrolyte.

As a rule, the minimum application of the fixing agent according to the present invention takes place with the aid of machines Application and dosing systems take place in which the chemical solution is finely distributed on the uniformly

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passing fibrous material in contiguous, the "The layer is sprayed or foamed onto the printed surfaces and that under neutral or weak acidic conditions preprinted textile goods here 12 to 40 ^ (based on the weight of the dry fiber material) the fixer takes up. The equipment requirements for a minimum order with this orientation are for example rotatable liquid spray heads or rollers, doctor blades, foam chambers or Gears met.

The preferred minimum application device for aqueous liquors is a spray unit is used, which sprays the fixing liquors on the textile material via rotors that with a speed of 3000 to 7000 rpm, preferably 5000 rpm, work and a spray width of 5 to 20 cm, preferably 10 cm, per rotor. At the specified speeds (revolutions per minute) the sprayed Fixing liquor with great force also pressed into the interior of very voluminous textile materials - e.g. knitted fabrics, as a result of the mentioned depth effect, a good levelness and coloration is achieved. In accordance With the width of the textile, the necessary number of rotors is placed side by side on a rotor arm arranged.

Instead of spraying, in the case of the application of chemical solutions of the type mentioned, the minimum application of fixing agent can be used furthermore also means based on the functional principle or the effect of rollers and / or doctor blades Measures take place. A wide variety of roller application systems are also suitable for thinner goods Squeeze joints, including rubber or steel rollers, magnetic squeegees with or without a metering device, coating squeegees or round stencils. Saddle rolls to which a scraper is pressed can also be considered.

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An interesting further development of such minimal application techniques is the application of foamed liquors, i.e. the replacement of a large part of the water in the treatment liquids through air. The wetting of the textile material takes place here through the large surface of the Foam.

The foams can be applied according to the invention claimed processes take place according to different technologies. The foam can either be opened by unrolling, Squeezing, sucking through, indirect doctoring, padding as well as using slot nozzles, rotary stencils, foam chambers or according to the principle of a gear pump by means of gear wheels with controllable speed on the textile material be applied.

According to the present invention, the amount of fixing solution applied is $ 12 to $ 35, preferably $ 15 to 25 for keratin fibers, and $ 15 to $ 40, preferably $ 20 to 30, for mixtures of keratin and cellulose fibers . The steaming time in the hanging loop damper is 4 to 16 minutes, preferably 6 to 12 minutes at 102 ° to 115 ° C. The quality of the steam is important here. "Moist saturated" steam is ideal for the perfect fixation of reactive dyes on wool.

Practically all commercially available dyes are suitable as reactive dyes for the new two-phase long steaming process Products with dichloro- and monochlorotriazine, di- and trichloropyrimidine, dichloroquinoxaline, dichloropyridazine, Difluorochloropyrimidine, monofluorotriazine, fluorochloromethyl pyrimidine, Vinyl sulfone, acrylamide and ethyl sulfonamide groups (Anchoring) as a fiber-reactive system.

The method according to the present invention is for the fixation of prints with reactive dyes on web-conveying

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moderate keratin fiber materials as well as their mixtures with cellulose fibers in all processing stages, such as fabrics, Knitted or nonwovens provided.

The following examples serve to illustrate the invention. The percentages given are by weight percentages and are based on the weight of the dry goods in the case of the data for the liquor pick-up.

example 1
50 g of the dye Reactive Black 5 (CI. No. 20 505) are mixed with

338 g of hot water dissolved and the resulting
Solution is in

600 g of an emulsion thickener stirred in, which in the

is available in the manner indicated below. Then you give the print paste prepared in this way
10 g of sodium 3-nitrobenzenesulfonate and
Add 2g of monosodium phosphate.

The aforementioned emulsion thickener is made as follows:

390 g of an oily, aqueous kernel meal ether thickener
5 will be with

130 g of a 10bigen, aqueous alginate thickener,
260 g water and

70 g of a 10bigen aqueous solution of a condensation product of polyglycol of mol. 2000 and
Mixed stearic acid.

This approach will be followed
150 g heavy petrol emulsified.

A fabric made of chlorinated wool is then printed with this printing paste using rotary film printing and dried. Then the current, the alkali-free form
having a web using liquid spray heads that rotate at approx. 5000 rpm, with a liquor pick-up of 15 $> sprayed with an alkaline solution which, in addition to water, consists of 150 g / l sodium acetate trihydrate and 50 g / l table salt. To fix the dye, the textile material is now steamed for 12 minutes at 102 ^° C. in a hanging loop damper. Afterwards, the printing inking produced is first rinsed with cold water as usual, then im
aqueous bath at 70 "to 80" C with 1 g / l of a commercially available detergent and 2 ml / l ammonia (25 #ig)

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pH 8 - 8.5 post-treated, finally rinsed again, acidified and dried.

A black print with good fastness properties is obtained.
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Example 2

40 g of the dye Reactive Orange 13 are dissolved in 348 g of hot water and the resulting solution is while stirring with

600 g of the emulsion thickener described in Example 1 are mixed. Then you add the printing ink preparation
10 g of sodium 3-nitrobenzenesulfonate and

Add 2 g of monosodium phosphate.
15th

With the printing paste created in this way, a knitted fabric made of chlorinated wool is now printed with film printing and this form is then sprayed with an aqueous solution using liquid spray heads rotating at approx. 5000 rpm with a liquor pick-up of 25 #, which contains 200 g / l contains sodium acetate trihydrate. For dye fixation is attenuates the thus treated textile material 8 minutes at 11O ⁰ C and treated as the print color produced in Example 1 given after.

An orange-colored print with good fastness properties is obtained.

Example 3

60 g of the dye Reactive Red 151 are dissolved with the help of 428 g of hot water and, with careful stirring, in 500 g of a 4% aqueous solution of a sodium alginate entered. Then you give the so prepared printing ink still

10 g of sodium 3-nitrobenzenesulfonate and Add 2g of monosodium phosphate.

With this printing paste, a fabric made of chlorinated wool is printed in roller printing and dried. The preprinted textile material is then sprayed with an alkaline solution using liquid spray heads rotating at approx. 6000 rpm with a liquor pick-up of 20 $> , which, in addition to water, consists of 130 g / l sodium acetate trihydrate and 100 g / l table salt consists. The dye is then fixed on the wool fiber by treatment with saturated steam for 10 minutes at 105 ° C. in a hanging loop steamer and the dyeing is finally aftertreated as indicated in Example 1.

A red print with good fastness properties is obtained.

Example 4

40 g of the dye Reactive Blue 166 are poured over with

448 g of hot water are dissolved and the resulting solution is dissolved in 500 g of a 10% aqueous solution of a sodium alginate stirred in. Then 10 g of sodium 3-nitrobenzenesulfonate are added to the printing paste Add 2 g of monosodium phosphate.

With this printing paste, a fabric made of chlorinated wool is then printed with film printing and dried. Separately from this, a 5 $ foam is produced, the per liter of aqueous liquor content
120 g sodium acetate trihydrate,

2 g of a surfactant mixture from approximately equal proportions Alkene sulfonates and hydroxyalkane sulfonates and, as a foam stabilizer, small amounts of a fatty alcohol, e.g., lauryl alcohol

contains. This foam of the weakly alkaline fixing agent is then used with a commercially available With the help of gears working application unit an even layer on the above-mentioned form of the alkali-free printing ink applied, its thickness

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in terms of quantity corresponds to a fleet pick-up of $ 20. The fabric treated in this way is then subjected to the action of steam at 103 ° C. in a loop damper for 12 minutes in order to bring about the dye fixation and finally post-treated as indicated in Example 1 and finished.

A blue print with good fastness properties is obtained.

Example 5

40 g of a green reactive dye mixture based on a metal-containing phthalocyanine-azo compound according to Example 3 of the German Offenlegungsschrift DE-A-27 45 480 are treated with 348 g of hot water are dissolved and, with stirring, in 600 g of an emulsion thickener according to Example 1

registered. Then 10 g of sodium 3-nitrobenzenesulfonate are added to the printing paste mixture

Add 2 g of monosodium phosphate.
20th

With this printing paste, a fabric made of deboned natural silk is printed with film and dried. An aqueous fixer solution containing 150 g / l sodium acetate trihydrate and 50 g / l Glauber's salt is then applied to the alkali-free pre-pressure created in this way by means of a roller against which a scraper is pressed, with a liquor pick-up of 20 $ . The goods covered in this way are then exposed to saturated steam in a hanging loop damper at 105 ° C. for 10 minutes and finished as indicated in Example 1.

A green print with good fastness properties is obtained.

Example 6

50 g of the dye Reactive Blue 21 are dissolved with 438 g of hot water and this solution is used

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with good mixing
500 g of a 4% aqueous solution of a sodium alginate

loaded. Then 10 g of sodium 3-nitrobenzenesulfonate are added to the printing ink Add 2g of monosodium phosphate.

With the printing paste prepared in this way, a chlorinated mixed fabric made of wool / cotton (60:40) is now im Rotary film printing printed and dried. On the so obtained Preprint with the alkali-free dye preparation is then made using a commercially available Dosing squeegee foulards by means of a magnetic bar pressed on, engraved doctor blade applied an aqueous solution containing 150 g / l sodium acetate trihydrate, 50 g / l soda and 50 g / l table salt. Here is a liquor pick-up set by 35 #. Used to fix the dye the printed textile material is then treated for 6 minutes with saturated steam at 103 ° C. in a loop steamer and finally post-treated as usual.

A turquoise-blue print with good fastness properties is obtained.

Claims (2)

Claims; . Process for the continuous fixing of prints with reactive dyes on textile webs made of keratin fibers or their mixtures with cellulose fibers by a two-phase steaming technique, the dissolved alkaline fixatives in the form of minimal amounts of liquor on the unfixed, beforehand with the reactive dyes Fiber material printed and optionally dried without the addition of alkali and hygroscopic agents is applied, characterized in that aqueous solutions of sodium acetate trihydrate, optionally mixed with other alkalis and electrolytes, and the impregnation process to cover the form with this fixing liquor either as such or in a foamed state by means of an application measure that brings about the uniform application of small amounts of liquid (minimum application) undertakes, and that the subsequent heat setting of the print on the so treated Textile material is brought about by long-term steaming in a hanging loop damper with saturated steam. 2. The method according to claim 1, characterized in that the minimum application of the fixing liquor with the aid of rotating liquid spray heads or rollers, doctor blades, foam chambers or gears as automated application and dosing system. 3- The method according to claim 1 or 2, characterized in that that the minimum order a liquor pick-up of the textile goods of 12 to 40 $ (based on the weight of the dry goods) on the fixing liquor. .G. HOE 4. Process according to Claims 1 to 3, characterized in that the prints are fixed in a hanging loop damper at 102 ° to 115 ° C over a period of 4 to 16 minutes. ORIGINAL ^r ^.