DE2604913A1 - Dyeing of synthetic fibres with disperse dyes - by addn. of acid donor to bath contg. soluble salt of dye - Google Patents

Abstract

Colouration of hydrophobic synthetic fibres involves conversion of a alt of a disperse dye contg carboxyl gps. to the free acid. This is achieved by addn. to the dyebath of an acid donor which becomes effective under dyeing conditions. Used for dyeing of synthetic fibres, e.g. polyester, polyamide or triacetate, by a discontinuous process. Use of a soluble dye salt and an acid donor results in slow pptn. of the dye acid during dyeing and greatly imporved results are obtd. In an example a satisfactory dyebathfor polyester fabric contained 5 wt. % on fabric of a mixt. of 100 pts. wt. anthraquinone dye salt and 55 pts. wt. Et diglycol and 2g/litre Na lauryl sulphate at a liquor ratio of 20:1. 3 wt.% of triMe phosphate was added as acid donor and dyeing was carried out at 120 degrees C.

Description

Process for dyeing synthetic fiber materials

The invention is a discontinuous process for Dyeing of synthetic hydrophobic fiber materials.

It is known that such fibers are normally coated with disperse dyes colored in very finely divided form.

A sufficient fine distribution of the predominantly water-insoluble To obtain dye particles, the dyes often have to be ground several times and are mixed with large amounts of dispersants. The dispersants used are intended to keep the dye in suspension until it is absorbed onto the fiber material and prevent agglomeration of the dye particles.

The production of such formed dye preparations is a relative one laborious, costly operation. In addition, the dispersants can be applied to the different dye types respond differently and therefore there will be different Special formations necessary.

In addition to the amount of dispersant, it is also often recommended to use the formed Dye preparation to add additional dispersant to the dyebath to prevent dye precipitation and avoid the resulting dye deposits and unevenness.

In addition to the considerable amount of work that the dye formation caused, as well as the resulting costs, represent the dispersant, which after all usually make up more than 50% by weight of the dye preparations and also in concentration of approx. 1 g / l are added to the dyebath, a considerable burden on the waste water represent.

In order to overcome these drawbacks, it has already been proposed (cf. DT-OS 2,317,946, 2,317,947 and 2,338,816), the formation of disperse dyes to save by using a water-soluble salt of a carboxyl group-containing The dye dissolves in the aqueous liquor and the dye through before the dyeing process Addition of acids in the dye liquor fails.

This procedure facilitates the production of the dye preparations, since the dissolving and replenishing of the dye are not laborious operations represent, however, this staining method leads to considerable problems, if at the moment the dyebath is acidified, the dye salt dissolved up to that point precipitates suddenly as an insoluble disperse dye.

If the precipitated dye also tends to agglomerate, so can do this, especially when dyeing cross-wound bobbins or densely packed material, easily lead to deposits and unevenness.

It has now been found that these dye precipitations can be prevented can, if you add acidic agents to the liquor, which only in the respective The area where the dye is absorbed onto the corresponding fiber becomes effective and gradually the dye salt in the disperse dye containing free carboxyl groups convict.

Because the "release" of the dye into the dyeable form is relatively slow takes place and the drawing of the same onto the fiber runs parallel to it, as well as the free carboxyl group-containing dispersion dye at higher temperatures (70-1400C) has a certain solubility, lies during the entire dyeing process a quasi-clear color liquor. Consequently, it does not occur with this approach to precipitations or to unevenness due to deposits of dye agglomerates.

The present method is also compared to the conventional one Dyeing with disperse dyes is relatively straightforward as it is less sensitive on fluctuations in the temperature control or on running through the The heating-up phase reacts. The acid donor can be added before, during or after Addition of the fiber materials take place.

Very good results are also obtained when using the dye liquor preheated and the dye preparation with the acid donor only at the final dyeing temperature is admitted.

As acid-releasing agents, derivatives are organic or inorganic Acids used that are specific only under the conditions as they are in the course of the respective fiber and dye-dependent absorption area in the dyebath present, release acidic groups and thus the pH value is neutral at the beginning or alkaline dyebath in the acidic range (preferably about pH 4.5).

Suitable means are for example; Esters, preferably C1-C4 alkyl esters of phosphoric acid, phosphorous acid, phosphonic acid and phosphinic acid, e.g. Trimethyl phosphate, triethyl phosphate, dimethyl phosphite, diethyl phosphite, trimethyl phosphonopropionate Suitable are also chloracetamide, the alkali and alkaline earth salts of mono- and dichloroacetic acid, preferably the sodium salt of monochloroacetic acid.

It is often appropriate to ensure that the textile material is evenly wetted and a commercially available wetting agent for the dye liquor to stabilize the dye solution to add.

The use of fatty alcohol sulfates is particularly advantageous here, preferably lauryl sulfate, in amounts of 0.5-4 g / l.

Suitable synthetic fiber materials produced by the new process can be colored are, for example (the temperature ranges are in brackets indicated in which the dyes are absorbed): Cellulose-2 1/2-acetate (70- 850C) Polyamides (80-100 ° C) cellulose triacetate and aromatic polyester (90-1400C) also Mixtures of these fibers and mixtures with hydrophilic natural fibers, such as Cellulose come into consideration.

The carboxyl group-containing dyes can be very diverse Belong to classes of substances, preferred are azoantquinone and quinophthalone dyes. Suitable dyes are, for example, in the above-mentioned patents and in GB-PS 489 698, 901 621, 963 816, in DT-OS 2 139 449, in DT-PS 1 266 272 and 1 469 732 described.

Suitable alkaline agents with which the dye-carboxylic acids converted into the water-soluble salts or those in the aftertreatment of the dyeings used to remove unfixed dye from the surface of the fiber material are metal hydroxides, such as sodium and potassium hydroxide, alkali metal carbonates, such as sodium and potassium carbonate and bicarbonate, alkali salts of inorganic Acids such as sodium borate, sodium silicate and trisodium phosphate, ammonia, organic Amines, such as triethanolamine, quaternary ammonium hydroxides and heterocyclic bases, which are made more hydrophilic by alkoxy solution (e.g. reaction with ethylene oxide) can.

The dyes can be in the form of their defined salts, e.g.

in the form of the sodium salt. Then theoretically that is sufficient stoichiometric amount of acid donor (based on the number of carboxyl groups. In practice, however, it is advisable to use an excess of 10-20% acid donor.

But you can also prepare the color salt solution in such a way that the dye carboxylic acid with preferably excess (10-100%) alkaline Brings funds into solution, but then has to have a correspondingly larger amount of acid donor use, so that at the end of the dyeing process a pH value below 7, preferably 4.5 sets.

The method according to the invention is based on the following examples explained in more detail, where "parts" mean parts by weight.

Example 1 10 parts of the carboxyl group-containing anthraquinone dye (According to DOS 1 932 828, p. 7) are reacted with 35 parts of a product which is prepared from 1 mole of triethanolamine with 3 moles of ethylene oxide. Of the dye preparation made up to 100 parts with 55 parts of ethyl diglycol, 5%, based on the weight of the polyester fabric to be dyed, are added to the dyebath together with 2 g / l of lauryl sulfate.

Add 3% by weight of trimethyl phosphate to the dyebath as an acid donor added. A liquor ratio of 1:20 is used for dyeing.

In the HT dyeing machine, in which the polyeater material is in constant motion and / or a sufficiently high circulation of the dye liquor must be guaranteed the liquor with a heating rate of up to 10 ° C / min to 120 C and 30 minutes colored at this temperature. After dyeing, it is washed and dried at approx. 600C, Small amounts of soda (approx. 2 g / l) can be added to the washing liquor.

A blue coloration is obtained, which has good all-round fastness properties characterized by excellent levelness and coloration.

Instead of the trimethyl phosphate used in the above example, 4% of the sodium salt of chloroacetic acid can also be used.

Example 2 A dye preparation is made from 20 parts of the following diphenylamine dye (According to DOS 1 932 828, p. 27) 35 parts of an amine compound from 1 mole of triethanolamine and 3 moles of ethylene oxide and 55 parts of ethyl diglycol.

In an HT dyeing machine that contains a device that enables to smuggle additives into the dye bath at dyeing temperature, polyester fabric is in a liquor ratio of 1:20 so colored that the aqueous liquor that only Contains 2 g / l lauryl sulphate, heated to 1300C in the dye container as quickly as required and at this temperature 6 wt .- $ of the dye preparation described above, as well 5% by weight of trimethyl phosphate are added.

It is 30 minutes at 1300C with sufficient agitation of the polyester material or / and dyed a sufficiently large liquor circulation, then drained the liquor and washed in a fresh bath at 600C and dried.

The result is a strong yellow color, which is next to a very good light fastness is characterized by good levelness and coloration.

The same results are obtained if, instead of the trimethyl phosphate, the same amount of chloroacetamide or can be used.

Example 3 Polyester fabric is dyed discontinuously in a liquor ratio of 1:10 under HT conditions, namely 12% by weight of a dye preparation was composed of: 10 parts of the following carboxyl group-containing anthraquinone dye (Can be prepared according to DT-PS 8 447 773) 35 parts of the amine compound of Examples 1 + 2, 55 parts of ethyl diglyco; together with 10% by weight of the sodium salt of chloroacetic acid and 2 g of lauryl sulfate are added to the dyebath and heated to 1200C with sufficient agitation of the polyester material orX and sufficient liquor circulation and left at this temperature for 30 minutes.

The liquor is then cooled, drained and rinsed at 60 ° C, then dried.

In this way, a brilliant red color is obtained, which is next to excellent lightfastness characterized by good levelness and color penetration.

A similar result is obtained if instead of the sodium salt the chloroacetic acid 6 wt .-% trimethyl phosphate are added to the dyebath.

Example 4 0.2 parts of the following dye (DT-PS 1 469 732, gap 23/24) are dissolved in a thread of 500 parts of water which contains 0.7 parts of the amine compound described in Example 1 and 1 part of lauryl sulfate.

After adding 1.3 parts 50 parts of a fabric made of 2 1/2 acetate are dyed in this liquor in such a way that, with sufficient movement of the fabric and / or sufficient liquor circulation, the dyebath is heated to 850C and dyed at this temperature for 1 hour. It is then rinsed and dried.

In the case of dark tones, a treatment with 1 part soda and 500 parts water are done at 600C to remove unfixed dye to be removed from the surface of the goods.

A level red dyeing with good in-use fastness properties is obtained good coloration.

Example 5 0.3 part of the following dye (according to DT-PS 1 469 732, column 23/24) are dissolved in a dyebath of 500 parts of water which contains 1 part of the amine compound described in Example 1 and 1 part of lauryl sulfate. After adding 2 parts of diethyl phosphite and 2 parts of o-creotinic acid methyl ester emulsified with 0.2 part of emulsifier W, 50 parts of a fabric made of triacetate are in this liquor in a dyeing machine with sufficient movement of the material to be dyed and / or sufficiently large liquor circulation Heated to 100 ° C. and dyed at this temperature for 1 h.

It is then rinsed and dried.

In the case of dark tones, a treatment with 1 part soda and 500 parts water are made at 70-800C to make unfixed dye to be detached from the surface of the goods.

A yellow dyeing with good lightfastness and good fastness properties is obtained.

Example 6 0.6 part of the following disperse dye containing carboxyl groups (Can be prepared according to DT-PS 8 447 773) are dissolved in the dyebath of 100 parts of water which contains 2 parts of the amine compound described in Example 1 and 1 part of lauryl sulfate.

Another 3 parts of dimethyl phosphite are added on a laboratory dyeing machine 50 g of a fabric made of polyamide in this liquor slowly with good liquor circulation heated to 1000C and dyed at this temperature for 30 minutes.

It is then rinsed and dried.

A brilliant red coloration is obtained, which is achieved with sufficient fastness properties characterized by good color penetration and levelness.

Claims (10)

Claims 1) Process for dyeing synthetic hydrophobic Fiber materials, characterized in that they are obtained from an aqueous solution of a salt of a disperse dye containing carboxyl groups with an acidic agent that only becomes effective under dyeing conditions, which is able to convert the dye salt into the free carboxylic acid, added. 2) Method according to claim 1, characterized in that the acid-donating Agent in the temperature range from 70 to 1400C is effective. 3) Method according to claim 1, characterized in that the acid-donating Agent is used in such amounts that a pH value is reached at the end of the dyeing process below 7, preferably 4.5, sets. 4) Process according to claim 1, characterized in that one ester phosphoric acid, phosphorous acid, phosphonic acid or phosphinic acid as acid donors used. 5) Method according to claim 1, characterized in that one chloroacetamide or alkali or alkaline earth salts of mono- or dichloroacetic acid as acid donors used, 6) Method according to claim 1, characterized in that that the acid donor is only added at dyeing temperature. 7) Method according to claim 1, characterized in that the dye liquor contains a wetting agent, preferably a fatty alcohol sulfate. 8) Method according to claim 1, characterized in that one is used for Formation of the color salts uses alkoxylated amines. 9) Method according to claim 1, characterized in that one polyester used as fiber materials and dyes at 90-140, preferably 100-1300C. 10) Synthetic fiber materials dyed according to the method of claim 1.