DE2521106B2 - METHOD OF DYING MATERIALS CONTAINING SYNTHETIC FIBER - Google Patents

Description

The present invention relates to a new method for dyeing synthetic fibers containing Materials, the dye liquor suitable for carrying out this process and the dye liquor according to the process or fiber materials dyed by means of the dye liquor.

When dyeing textile material with dyes that are insoluble or sparingly soluble in water, for example with the so-called high-temperature circulation dyeing process, dispersion difficulties often arise which can be attributed to insufficient fine distribution of the dyes in the dye liquors. This results in uneven and false, especially non-rubbing, dyeings. Such defects are noticeable, among other things, when dyeing synthetic fibers, especially linear polyester fibers, with disperse dyes,
ίο As is well known, one can for the stability of the dispersions of dyes that are sparingly soluble in water certain B. condensation products of naphthalenesulfonic acid with formaldehyde or their Alkali.valze. oxyethylated fatty alcohols or lignosulfonates.

However, these products either have only dispersing or only leveling properties. Both effects can therefore almost only be achieved by using a mixture of different aids.

zo ifl. Many dispersants also affect the dispersing and coloring process due to their strong tendency to foam.

A new method has now been found which allowed when dyeing synthetic fiber-containing materials mi sparingly soluble to insoluble in water To obtain dyes level and rub-fast colorations. The new method consists in that one , Fibers in the presence of a water-soluble, sulfo-containing Polyadduct of propylene oxide with a polyvalent, at least 2 carbon atoms and preferably 3 to 6 carbon atoms containing aliphatic alcohol.

With the aid of the above-mentioned anionic polyadducts, those described at the outset can now be achieved Eliminate the disadvantages of dyeing organic synthetic fibers, especially polyester fibers occur with the disperse dyes without additives or with the previous additives. Of the Technical progress achieved according to the invention is based primarily on the excellent dispersion-stabilizing properties Effect of the polyadducts on the dye, so that during the entire dyeing process neither one Aggregation or precipitation of the dye takes place.

Another advantage of these compounds used as leveling and dispersing agents lies in the low tendency to foam. There is therefore no risk of foam spots forming on the Dyeings and thus a faster penetration of the goods and an increase in the flow rate guaranteed in the dyeing machines.

The polyadducts used according to the invention are, for example, with Using a sulfonated organic, preferably aliphatic, mono- or dicarboxylic acid from 3 to 6 Carbon atoms such as B. propionic acid or succinic acid, but preferably by using a inorganic sulfating agent, in particular sulfuric acid or sulfamic acid, into an acidic ester transferred addition products of propylene oxide to at least 2, preferably 3 to 6 carbon atoms containing polyhydric aliphatic alcohols.

Polyhydric alcohols according to the definition are those which contain at least 2 hydroxyl groups

<, _s pen have, for example alkylene diols with an alkylene radical of 2 to 6 carbon atoms, such as. B. ethylene glycol, 1,3- or 1,2-propylene glycol or 1,5-pentanediol, glycerol or trimethylolpropane. Loading

25th 1 / \ f *

ι KJ υ

Preference is given to using aliphatic alcohol «, which three carbon atoms and two or three hydroxyl (i groups exhibit.

For use according to the present invention, for example, sulfated ones according to the definition have been found Incorporated products, whereby the polyadduct is an average Molecular weight from 1000 to 6000, preferably from 2000 to 3500, has proven particularly useful. Among these, addition products derived from propylene glycol or glycerine are particularly suitable.

Pie according to the invention to be used sulfo groups Polyadducts can be used as free acids or, preferably, in the form of their alkali metal or ammonium salts can be used. As alkali metal salts are in particular the sodium and potassium salts and as ammonium salts the ammonium, trimethylammonium, monoethanolammonium, diethanolammonium and called Triälh & nolammoniumsalzc. The polyadducts are preferably used as ammonium sulfate salts used.

Typical representatives of the present invention reaching the application sulfo-containing polyadducts rfind by reacting polypropylene glycol and sulfamic Umsetzungsprodiikt obtained, wherein jj _as polypropylene glycol having an average molecular weight of 1000 to 3500, preferably 2000 and the sulfated from glycerol or trimethylolpropane and propylene oxide adducts obtained with the Polyadducts have an average molecular weight of 2000 to 6000, preferably 3000 or 2500.

Another representative containing sulfo groups is the sulfo-succinic acid half-ester obtained by addition Polyadduct obtained from propylene oxide on glycerol, the half-ester having an average molecular weight of about 4000 has.

The amount of polypropylene oxide adducts containing sulfo groups move according to the present invention between 0.1 and 5 g, preferably 0.5 to 2 g, per liter of the aqueous dye liquor.

It is often desirable to incorporate an antifoam agent into the aqueous solution of the polyadduct in order to to improve the properties of the dyebath to which the dispersant is added and sometimes also to increase the migration of the dye. A satisfactory type of antifoam agent is one Silicone emulsion, for example a 5 to 10% aqueous silicone emulsion, which can also be used in combination with higher alcohols of 4 to 22 carbon atoms, in particular with 2-ethylhexanol, can be used can. However, the most suitable antifoam agents are water-insoluble alkylene oxide adducts of higher alcohols for example the adduct of stearyl alcohol and 1 mole of ethylene oxide, as well as esters of aliphatic Dicarboxylic acids and higher alcohols or the higher alcohols alone, e.g. butyl alcohol or 2-ethylhexanol.

Adipic acid di-2-ethyl-hexyl ester has proven to be particularly suitable as well as methylpolysiloxane proved. 6q

The amount of antifoam used can already be, for. B. 0.5 weight percent, but with advantage at least 10 percent by weight, preferably 15 to 60 percent by weight, based on the weight of the Polyadducts. (^

You can also add water-miscible alcohols to the solution of the polyadduct. Suitable for this in particular lower aliphatic alcohols such as

Alkanols, z, B, ethyl alcohol, n · and iso-propyl alcohol, tfirt. Butyl alcohol, alkylene glycols e.g. ethylene glycol and 2,5-hexanediol and their lower monoalkyl ethers, as well as their mixtures,

For the purposes of the invention, dyes that are insoluble or sparingly soluble in water include vat dyes, PigiTtientfarbsioffc and especially disperse dyes to understand, which are laser-affine, d. H. such, wekhe on laxtilc synthetic fiber materials

These dyes can belong to a wide variety of classes, e.g. B. amido dyes, nitro dyes, Methine and polymethine dyes, styryl and azosiyryi dyes, Xanthene dyes, oxazine dyes, aminonaphthoquinone dyes, Coumarin dyes and in particular anthraquinone dyes and azo dyes such as monoazo and diazo dyes.

Mixtures of such dyes can also be used according to the invention.

The method according to the invention is also suitable for tinting undyed textile materials with in white Water slightly soluble optical brighteners. These can belong to any class of brightener. In particular it is stilbene compounds, cuinarines, benzocumanne, pyrazines, pyrazolines, oxazines, Triazolyl, denzoxazolyl, benzofuran or benzimidazolyl compounds and naphthala auramides.

The amount of the process according to the invention | the dyes added to the liquor depends on the desired color strength; in general have ' Quantities of 0.01 to Iu percent by weight, based on the fiber material used, have proven useful.

As fiber materials that can be dyed according to the invention, cellulose ester fibers, such as cellulose-2 ^! // - acetate fibers and triacetate fibers, synthetic polyamide fibers, e.g. B. those from ε-caprolactam, from adipic acid and hexamethylenediamine, from ω-aminoundecanoic acid, polyurethane, polyolefin fibers, z. B. polypropylene fibers, polyacrylonitrile fibers, including modacrylic fibers and especially linear polyester fibers to be mentioned. Linear polyester linear polyester fibers are to be understood as synthetic fibers obtained by condensation of terephthalic acid with ethylene glycol or of isophthalic acid or terephthalic acid with 1,4-bis (hydroxymethyl) cyclohexane, as well as copolymers of terephthalic acid and isophthalic acid and ethylene glycol. The fiber materials can also be used as mixed fabrics with one another or with other fibers, e.g. mixtures of polyacrylic / polyester. Polyamide / polyester, polyester / viscose and polyester / wool can be used.

'The fiber material can be present in a wide variety of processing stages, e.g. B. in the form of Flakes, piece goods, such as woven and knitted fabrics, yarn bundles, wound bodies, as nonwovens, textile Flooring or tufted carpet.

The dyeings are advantageously carried out from aqueous liquor using the exhaust process. Linear polyester fibers are preferably dyed by the so-called high-temperature process in closed and expediently also pressure-resistant apparatus at temperatures of over 100 ^° C., preferably between 110 and 140 ^° C., and optionally under pressure. Circulation apparatus such as cross-bobbin or tree dyeing systems are suitable as closed vessels. Reel skids, nozzle or drum dyeing machines, paddles or jiggers. The liquor ratio can accordingly be within a wide range

be chosen, ζ. B. 1: 1 to I: 100, preferably 1; 10 to 1: 50 The coloring of the linear polyester fibers may also at temperatures below 10O ⁰ C. z, B, in the temperature range 75-98 ⁰ C ₁ in the presence of the usual color carrier (carriers), such as phenylphenols, polychlorobenzenes, xylenes, toluenes , Naphthalenes or diphenyl. Cellulose 2> / 2 acetate-man while Zellulosetriacetatfascrn be dyed with advantage at the boiling point (98 ⁰ C) of the aqueous bath preferably dyed at temperatures of 80 to 85 ⁰ C.

When dyeing cellulose-2 '/ i-acetate' or polyamide fibers, there is no need to use dye carriers. In the preparation of the dye liquors, it is expedient to start from the aqueous solutions of the polyadduct and to add suitable auxiliaries such as antifoams and lower alcohols to them. The liquors can contain mineral acids such as sulfuric acid or> λ ^ preferably phosphoric acid, organic acids, ^ j ^ «appropriately lower aliphatic? Carboxylic acids such as formic acid, acetic acid or oxalic acid and / or salts such as ammonium acetate, ammonium sulfate or sodium, / acetate. The acids mainly serve to adjust the pH-value of the present invention, "% ^ usable fleets of, usually 4 to 8

'is preferably 4.5 to 6.5.

'"Ί You enter the liquor with the textile material, the

may have a temperature of 40 to 7O ⁰ C, and the material -behandelt 5 to 15 minutes at this

, {Temperature. Then you give the dye and

if necessary, the carrier and increases the temperature the liquor to dye in the specified temperature range for 50 to 100 minutes.

e _L The dyed material is then rinsed and dried as usual. A reductive follow-up treatment is normally not necessary. As a rule, the material to be dyed rests in the dyeing machine and the liquor circulates through the material to be dyed. It is important that there is not only a dispersion of the dye initially, but that the degree of dispersion is maintained throughout the dyeing process.

As is well known, certain disperse dyes tend to, especially under the conditions of high temperature

"dyeing to pass into a more fine form. The The consequence of this is that the dye is no longer absorbed onto the fiber and adheres to the surface of the Dyed goods settle. Such dye agglomerations and deposits can be caused by the invention Avoid using anionic polyadducts particularly well.

According to the invention, the synthetic fiber material also continuously, d. H. by impregnation with an aqueous preparation containing a disperse dye, contains a defined anionic polyadduct and optionally a thickener and acid, and squeezing to the desired content of impregnating liquor of 60 to 120% of the fiber weight with subsequent heat treatment, such as B. Steaming at temperatures from 98 to 105 ° C with neutral saturated steam or heat setting at 180 to 210 ° C.

According to the method according to the invention, one obtains on synthetic hem organic fiber material, esp. »Ondere on linear polyester fibers, uniform and strong colors, which are also characterized by good rub fastness and color yields.

In the preparation instructions and examples below, percentages mean percentages by weight and Parts parts by weight.

Manufacturing prescriptions

A 100 g of pure polypropylene glycol of average molecular weight 2,000 borrowed be heated to 6O ⁰ C. Then 20 g of urea and 20 g of sulfamic acid are added with stirring within 30 minutes. The mixture is stirred for a further 30 minutes at 60 to 65 ^° C., then heated to 95 ^° C. and held at 95 for 10 hours

ίο to 100 ⁰ C, to give a viscous yellowish product, which is completely soluble in water and contains 80% of the ammonium salt of the di-Schwefelsäureestcrs.

B. 62 g of the condensation product obtained from glycerol and propylene oxide of the average MoIe-

kular weight 3100 are added as described under A with 6.4 urea and 6.4 g sulfamic acid and esterified. A viscous product which is readily soluble in water and contains 92% of the ammonium salt of is obtained Contains sulfuric acid ester.

% A C, 75 g of the adduct of trimethylolpropane and propylene oxide with an average molecular weight of 2540 are reacted as described under A with 9.6 g of sulfamic acid in the presence of 9.6 g of urea. A viscous, in

Sulphated product which is readily soluble in water.

D. 100 g of an iviüieinsäurehalbesters of the formula

CH ₂ -OJ-CH CH ₂ ο

COC ¹ H CHCOOH

CH-O

CH ₂ -O-

-CH-CH, - O ^ -COC ^- M CH-CO (JH

CH,

-CH CH,
CH,

I "2

-COCH = CH-COOH

πι + / 72 + m = about 63, molecular weight about 4000, are stirred with the addition of 7.12 g of sodium metabisulfite in 400 ml of water for 9 hours under reflux, the pH of the reaction mixture using 7.5 ml of a 10% aqueous sodium hydroxide solution is kept between 5.5 and 6.5. The result is a pale yellowish, opal solution, which has a degree of attachment, determined via the non-reacted sulfite content, of 100%. After evaporation at 40 to 50 ⁰ C to obtain 109 g of the sodium salt of the sulfosuccinic monoester in the form of a hygroscopic s'trk sticky mass.

E. 100 g of the obtained from glycerol and propylene oxide condensation product of the average molecular weight of 4000 are heated to 6O ⁰ C. Then 10 g of urea are added in 15 minutes and 10 g of sulfamic acid in 30 minutes. After further stirring at 60 to 65 ° C for 30 minutes, heated to i00 ° C and holding for one hour at ICO ⁰ C and a further 9 hours at 105 C. The Sulfaiierungsproduk ^c "obtained is clearly soluble in Wgsser.

F. Proceed according to manufacturing instruction E. uses, however,! 0Og of a condensation product obtained from glycerol and propylene oxide

fts average molecular weight 6000.

G. lOCg polypropylene glycol of the average Molplinlargewirht 100Q are made in the same way as in manufacturing orschrift E with 40 g of sulfamic acid in

Esterified in the presence of 40 g of urea. The reaction product obtained contains 66% of the ammonium salt of the acid sulfuric acid ester and is clearly soluble in water.

H. 47.6 g of the adduct of 1 mole of ethylene glycol and 40 moles of propylene oxide of average molecular weight 2380 are in the same way as in preparation E in the presence of 8 g of urea Esterified with 8 g of sulfamic acid.

I. 40 g of the product obtained according to the manufacturing instructions are mixed with 10 g at 60 ° C Adipic acid di-2-ethylhexyl ester and then with 0.5 g of the adduct of 1 mol of castor oil and 40 mol of ethylene oxide, 3 g of water and 2.5 g of isopropanol mixed. A liquid, homogeneous product is obtained, v / obei after dissolving in Water of the adipic acid ester is present in a fine emulsion.

K. 37 g of the product obtained according to manufacturing method B are mixed with 3 g of monoethanolamine and then mixed with 50 g of benzene. Benzene and ammonia are then driven away in a vacuum, whereupon the Monoethanolamine salt of the acid sulfuric acid ester of the condensate of glycerol and propylene oxide from average molecular weight 3100 is obtained.

L. The procedure is according to manufacturing specification K, but 5 g are used instead of monoalhanolamine Triethanolamine. It becomes the corresponding triethanolamine salt obtain.

M. 50 g of the obtained according to manufacturing procedure B. 50 g of water are added to the product. 0.8 g of an aqueous solution are added to the clear solution obtained Mixing in an emulsion of methylpoiysiloxane.

example 1

25 g of a knitted fabric made of polyethylene glycol terephtha-Ia! are in a circulation stainer with a Liquor containing 0.6 g of ammonium sulfate and 0.3 g of an auxiliary gene,; sches consisting of 55 parts of the sulfuric acid ester obtained in accordance with the manufacturing specification B 10 parts of di-2-ethylhexyl adipate and 35 parts Water and iscpropaool (1 1) in 300 ml of water and is adjusted to pH 5.5 with 85% formic acid. Treated at b0 C for 10 minutes. Thereafter 1.35 g of a dye mixture consisting of 0.875 g of a dye of the formula are added to the liquor

Cl

and 0.475 "of a dye of the formula

OH

CO

H r H

! CO

• Md him / i die f-'iirhcflotie within 30 minutes

f3r

to 13O ⁰ C. The dyeing for 60 minutes at this temperature and cools the liquor at 90 ⁰ C from. The coloration obtained is rinsed and dried. The result is a rub-fast, brilliant red coloration.

Example 2

400 g of a wound body made of polyethylene glycol terephthalate fibers are placed in a circulation dyeing apparatus with a liquor which contains 16 g of the sulfonate obtained according to manufacturing instruction A dissolved in 8 liters of water and adjusted to pH 5.5 with 85% formic acid is treated for JO minutes at 6O ^{0 C.} Then ί g of a dye mixture consisting of 0.4 g of a dye of the formula are added to the liquor

NO ₂

Cl

N (CH ₂ CH ₂ CN) ₂
(3)

0.2 g of a dye of the formula

NO ₂

) ^ N (CH ₂ CH ₂ OCOCH ₃ ),
(4)

and 0.4 g of a dye of the formula
HO O NH,

35 H ₂ NO OH

and the dye liquor is heated to 130 ^° C. over the course of 30 minutes. It is dyed at this temperature for 60 minutes and then the liquor is cooled to 90 ^° C., after which the dyeing obtained is rinsed and dried. A level gray coloration is obtained.

Example 3

If the auxiliaries mentioned in Example 1 or 2 are replaced by the same amounts of one further auxiliary consisting of 80 parts of the sulfuric acid ester obtained according to preparation B and 20 parts of that made from stearyl alcohol and

1 mol of ethylene oxide obtained condensation product and the rest of the procedure as in Example 1 and 2 respectively indicated, level dyeings are also obtained.

Example 4

If you replace those in example 1 or 2 mentioned auxiliary by the same amounts of another auxiliary consisting of 60 parts of the sulfuric acid ester obtained according to preparation B and 40 parts of butyl alcohol and discolored in the

ho the rest as given in example 1 and 2, respectively you also have level dyeings.

Example

If you replace in example 1 or 2 in each case there

(, _s named auxiliary by the same amounts of a ' Auxiliary consisting of 80 parts of the sulfuric acid obtained according to preparation procedure B esters and 20 parts of a mixture of 5% silicone oil

609 525/430

and 95% 2-ethylhexanol and the rest of the procedure as in Example 1 and 2 given, level dyeings are also obtained.

Example 6

If, in Example 1, the mixture of auxiliaries mentioned there is replaced by 2.2 g of sulfuric acid ester obtained in accordance with Preparation C and 0.13 g Adipic acid 2-äthyIhexylester and proceeds otherwise as indicated in example 1, one also obtains! line legal coloring.

One arrives at similar results. if in place 4 of the aids received according to manufacturing specification C - "IeIs the sulfosuccinic acid half-ester obtained according to manufacturing specification D is used.

Example 7

Rubbing, level dyeings are also obtained if, in example 2, the product according to manufacturing instruction A by 8 g of the product according to the manufacturing specification ί every 16 g of the product according to manufacturing specification M © if the mixture of auxiliaries mentioned in Example 1 by 0.3 g of the product according to manufacturing instructions I or 0.6 g of the product according to manufacturing instructions M is replaced.

Example 8

Even colorations are also obtained with the products according to the manufacturing instructions E, F, G, H, K, L, if these in the corresponding amount instead of the product according to manufacturing specification B according to Example! 1 can be used.

Example 9

40 g of a fabric made of polyethylene terephthalate staple fibers are in a dyeing machine during

Colored, 0.5% (based on Stöffgewicht) of a 20% aqueous dispersion of the optical brightener of formula: -CH CH 16 minutes at 13O ⁰ C under agitation in a liquor (liquor ratio 1 9)

-CH = CH

CH,

and 5 g per liter of the preparation according to manufacturing ^ regulation I. The fleet is at 13O ⁰ C

15 *! Drained. The rinsed in the usual way and dried fabric shows a very high, brilliant lightening effect with a neutral shade and complete Equality. A coloration in which instead of 0.5 g of the preparation according to manufacturing instruction I

4.0 g of a 25% strength aqueous solution of the leveling agent the formula

? Cl7H35CH2O- (CH2-CH2O) 35-H

are used per liter, results in a significantly poorer brightening under otherwise identical conditions of insufficient equality. In some places there are even green discolorations on the treated tissue detected by undeveloped brighteners.

Example 10

A fabric made from polyethylene terephthalate staple fibers is padded in a liquor containing 5 g per liter of a 20% aqueous dispersion of the optical Brighteners of the formula

and 2.5 g of the preparation according to preparation I contains. (Squeeze off 50%). This will be fixed at 60 ⁰ C and then dried for 30 seconds at I9O ° C. A brilliant, very high lightening effect is obtained.

The same color, but without the addition of the preparation according to manufacturing specification I, provides a fabric that is only sufficiently lightened and greenish in color due to incompletely developed optical brighteners. When fully developed, but without reaching the effect of the product according Herstellürigsvor- "chrift I carried and fixed also at 21O ⁰ C lightening brighteners only at a fixing temperature of 210 ⁰ C.

In the same way, by using the product according to manufacturing instructions I, the fixing temperature a combination of the optical brighteners of the formulas

CH = CH

CN

and

CU, -C- ^ N

- - J

y (9)

can be reduced from 190 to 170 ^{1 C.} Example 11

'" 25 g of a knitted fabric made of polyethylene glycol terephthalate, wound on a perforated metal support, are in a circulation dyeing machine with a

Liquor containing 0.6 g of ammonium sulfate and 0.3 g of an auxiliary agent mixture consisting of 55 parts of the sulfuric acid ^{ester obtained in accordance with Hcrstelv "| s} y, ^{regulation B , 1} J; i ^e ! ^En ., ^Adi P'nsäuren-di-2- äthy! -hexylester and Jj parts of water and isopropanol (1: 1) and 1.5 g of one

ft contains ₅ Carriers of the type Trichlorbcnzol / Diphenyl in 300 ml of water and with 85% formic acid IGCR adjusted to pH 5.5, for 10 minutes at 60 ⁰ C treated Then one adds the fleet 0.625 g of a dye

25 21406

the formula

Cl

NO,

NH-CH ₂ CH ₂ OH

IO

to and the Fäi befloUe heated within 30 minutes to 98 ° C are dyed for 60 minutes at this temperature and then cool the liquor to 9O ⁰ C from. The coloration obtained is rinsed and dried. The result is a rubbing, level, brilliant, red coloration which does not show any dye deposits on the inside of the lap carrier.

Example 12

10 g of a fabric made of polyacrylonitrile are in a dyeing machine with a liquor containing 0.8 g of an auxiliary mixture consisting of 55 parts of the sulfuric acid ester obtained according to preparation B, 10 parts of di-2-ethylhexyl adipate and 35 parts of water and isopropanol (1: 1) in 400 ml of water and adjusted to pH 5.5 'with 80% acetic acid, ^{treated at 60 °} C. for 10 minutes. Then 0.05 g of a dye of the formula is added to the liquor

O NH-CH.,

(11)

NH -CH, CH, OH

ester and 35 parts of water and isopropanol (1: 1) in 200 ml of water and is adjusted to pH 5.5 with 80% acetic acid and which contains 0.05 g of the dye of the formula (11) used in Example 12, introduced . The dye liquor was then heated to 125 ° C. in the course of 45 minutes. Dyeing for 30 minutes at this temperature and then cools the fleet to 8O ⁰ C from. The coloration obtained is rinsed and dried as usual. The result is a rubbing, level, brilliant, blue coloration.

Example 14
0.1 g of a disperse dye oer formula

zo

to the dye liquor and heated within 30 minutes to 98 ° C are dyed for 60 minutes at this temperature and Viihli the liquor at 60 ⁰ C from. The coloration obtained is rinsed and dried. The result is a rubbing, level, light blue coloration.

Example 13

5 g of a fabric made of triacetate are in a high-temperature dyeing machine in a liquor containing 0.2 g an auxiliary mixture consisting of 55 parts of the sulfuric acid ester obtained in accordance with manufacturing specification B, 10 parts of adipic acid-di-2-ethyl-hexyl-

(12)

HO Ji NH-CH ₃
O

^Z 5 are dissolved in 300 ml of water which contains 0.15 g of an auxiliary mixture consisting of 55 parts of sulfuric acid ester obtained in accordance with manufacturing specification B, 10 parts of di-2-ethylhexyl adipate and 35 parts of water and isopropanol (1: 1), stirred in. Then, as is customary in dyeing, the liquor is heated to 98 ° C. within 30 minutes and kept at this temperature for 10 minutes. After cooling, the dye liquor was drained through a round filter to determine any dye agglomerations. The dye dispersion was even after this treatment still flawless, there were no agglomeration-related dye deposits.

Example 15

A fabric consisting of a mixture of polyethylene glycol terephthalate and wool (50:50) is placed in a dyebath with a liquor containing 0.8 g of ammonium sulfate and 0.8 g of an auxiliary mixture consisting of 55 parts of the sulfuric acid ester obtained in accordance with manufacturing specification B, 10 parts of ad'ipic acid di-2-ethyl hexyl ester and 35 parts of water and isopropari oil (1:!) In 400 ml! Water, and 0 (2 g of the disperse dye of the formula

HO-CH ₂ -CH ₂ -O

OCH ₃

- / \ -

OH

(13)

contains and is adjusted to pH 5.5 with 80% acetic acid, treated. Thereafter, the dye bath, under continuous movement of the tissue within 30 minutes 9S ⁰ C heated, dyed for 60 minutes at this temperature, then rinsed and dried as usual.

The fabric treated in this way shows a strong color Coloring of the polyester part and a clear reservation of the WoII part.

Example 16

Piece goods made of polyacrylonitrile are added to the padder with a liquor pick-up of! 00 percent by weight padded an aqueous liquor at room temperature, which contains per liter:. · '. < '

5 g of the disperse dye used in Example 12

fes of formula (II),

6 g starch ether,

<r

5g of the auxiliary agent mixture, consisting of 55 parts of the sulfuric acid ester obtained according to Preparation B, 10 parts of di-2-ethylhexyl adipate and 35 parts of water and isopropanol (l: 1)

and their pH is adjusted to 5.5 with acetic acid. The goods treated in this way are then left in a steamer for 30 minutes without drying Treated at 10 ° C (saturated steam). The "% are rinsed and dried as usual.

You get so
light blue coloring.

a brilliant, level, rub-proof,

17th

NH

R - O ₂ S

/ V-N - = N

NO,

example

10 g of a textured Polyäthyleiilerephthalatgewebes are in a dyeing machine with a liquor containing 0.24 g of ammonium sulfate and 0.24 g of the auxiliary agent according to preparation I in 120 ml of water and is adjusted to pH 5.5 with 85% formic acid, 10 minutes Treated at 6O ^{0 C.} Then the mixture is heated, the fleet over 35 minutes to 135 ⁰ C and then added 0.018 g of a dye of the formula "■■ '.

IR = CH ₃ and C ₂ H ₅ (I: 1)

ig of a dye of the formula

O ₁ N

IN THE-/

Cl

N - CH ₂ CH ₂ - O - CH ₂ CH ₂ CN
CH ₂ CH ₂ CN

and 0.015 g of a dye of the formula

NH - CH ₂ CH ₂ OCH ₂ CH ₂ CN

NHCOCH ₂ CH,

added. Dyeing for 30 minutes at this temperature and subsequently cooled down to 9O ⁰ C. The coloration obtained is rinsed and dried. A level, gray coloration is obtained.

Example 18

Textured polyethylene terephthalate fabric is impregnated with an impregnation liquor containing 29 g / l of a dye of the formula

10 g / l of an auxiliary agent according to manufacturing specification I,

2 g / l alginate thickener,
0.5 g / l sodium alkylnaphlhalinsulfonic acid and 2 g / l monosodium phosphate

NH ₂

-N -

and is adjusted to pH 6.5 with acetic acid. at 20 C. to 30 ° is then squeezed to 98%, based on the dry weight of the product from, trocknel at 12O ⁰ C for J tbermofixierl minutes and at 190 ⁰ C during 45 seconds. The dye is washed with it

((7j 50 cold water and dry. You get a level, red ■ coloring. If necessary, the 'usual

'■ fj.' Reductive post-cleaning carried out after rinsing

know.

Claims (12)

Patent claims: 1. Process for dyeing synthetic fiber-containing materials with heavy to in water insoluble dyes, characterized in that that the fibers in the presence of a water-soluble, sulfo-containing polyadduct of propylene oxide on a polyvalent aliphatic one having at least 2 carbon atoms Alcohol stains. 2. The method according to claim I, characterized in that that you have a water-soluble, sulfo-containing polyadduct of propylene oxide on a polyhydric alcohol containing 3 to 6 carbon atoms is used. 3. The method according to any one of claims 1 and 2, characterized in that the sulfo-containing Polyadducl a sulfuric acid ester of an addition product of propylene oxide on a polyhydric alcohol containing 3 to 6 carbon atoms. 4. The method according to any one of claims 1 to 3, characterized in that the polyadduct is a average molecular weight of 1,000 to 6,000, preferably 2,000 to 3,500. 5. The method according to any one of claims 1 to 4, characterized in that the polyadduct derived from propylene glycol or glycerin. 6. The method according to any one of claims 1 to 5, characterized in that 0.1 to 5 g, preferably 0.5 to 2 g of the sulfo-containing polyadduct is used per liter of dye liquor. 7. The method according to any one of claims 1 to 6, characterized in that the polyadduct combined with an anti-foam agent. 8. The method according to claim 7, characterized in that that as antifoam adipic acid-di-2-ethyI-hexyl ester is used. 9. The method according to any one of claims 1 to 8, characterized in that the dyeing is carried out by an exhaust process. 10. The method according to any one of claims 1 to 9, characterized in that as synthetic Fibers uses linear polyester fibers. 11. The method according to any one of claims 1 to 10, characterized in that the dyeing is carried out at a temperature of 110 to 140 ° C. 12. Fa: beflotte for dyeing synthetic fiber-containing materials, especially linear ones Polyester fibers, characterized in that they lift at least one heavy to in water insoluble dye a water-soluble, sulic group-containing Polyadduct of propylene oxide on a polyvalent one containing at least 2 carbon atoms, Contains aliphatic alcohol.