DE2056984A1 - Process for coloring textile material - Google Patents

Description

- ¹ ! ¹ :! Jilllfli! "!! '!!'": ¹ 1: ¹ ::? ■ "■■■■ '" ■: ■ "' ■ -. '« A

Case 690VE

Germany

Process for dyeing textile material.

The present invention relates to a method for dyeing organic, wide-spread textile material with a pronounced third dimension.

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The method according to the invention is characterized in that the broadly guided textile material subject to a treatment, which consists essentially of

a) Impregnation of the material with an aqueous dye liquor containing a fiber-affine dye and optionally a surface-active aid contains, and

b) treating the impregnated material in an aqueous bath during one for fixation of the dye for a sufficient period of time

and then finished by rinsing and drying.

As a textile material that is dyed according to the invention can be made from natural and synthetic fiber materials.

Among others: wool, silk, synthetic polyamides, especially poly (hexamethylene adipic acid amide), Poly- (ε-caprolactam), poly- (hexamnethylenesebacic acid amide), Poly (II-aminoundecanoic acid) or modified Polyamide fibers, such as acid modified polyamide, acrylic or acrylonitrile fibers, mixed polymers Acrylonitrile and other vinyl compounds such as acrylic esters, acrylamides, vinyl pyridine, vinyl chloride or vinylidene chloride; Polyester fibers such as high molecular weight esters of aromatic dicarboxylic acids with polyhydric alcohols, e.g., polyethylene glycol terephthalic acid esters; Polyethylene-polypropylene fibers, also cellulosic fiber materials such as tree

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wool., regenerated cellulose fiber, and cellulosed! - or -tria acetate fibers.

The textile materials can also be in the form of blended fabrics, for example made of different synthetic polyamides, made from wool and cellulose acetate, made of wool and polyacrylonitrile or wool and polyethylene glycol terephthalate fibers. Man at the same time dyes the different fiber parts with the appropriate dyes and thus maintains multi-colored patterned textile material.

The dyes with affinity for fibers that can be used can, depending on the substrate to be dyed, be water-soluble or else only be dispersible in water.

The water-soluble dyes are primarily those that reduce their solubility in water Owing to the presence of acidic groups, such as carboxylic acid groups, but in particular of sulfonic acid groups. Furthermore can they belong to the most diverse classes, such as e.g. those of the oxazine, triphenylmethane, xanthene, nitro, methine, quinophthalone, acridone or phthalocyanine dyes, but especially of the metallized and metal-free mono-, dis- or polyazo dyes and Anthraquinone dyes. Among the azo dyes mentioned those which contain a sulfonic acid group are preferred, in the case of the azo metal complexes it is those which have two azo dye molecules on one metal atom.

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Particularly suitable metal atoms are chromium and cobalt. These 1: 2 metal complexes can also do this be free of acidic groups and have alkylsulfone or sulfonamide groups in their place.

The water-soluble dyes mentioned can also contain reactive groups which are capable of entering into a chemical, that is to say covalent, bond with the textile material to be dyed. Groups which may be mentioned which give the dye this ability are: epoxy groups, ethyleneimine groups, isocyanate groups, aryl carbamate groups, sulfonic acid halide groups, vinyl sulfone groups and aliphatically bonded sulfuric acid ester groups or halogen atoms. These last-mentioned reactive substituents are expediently in the 7- or in the β-position of an aliphatic radical which is bonded to the dye molecule directly or via an amino, sulfonic acid or sulfonic acid amide group. Dyes which contain halogen atoms as labile substituents, for example bromine atoms, but preferably chlorine atoms, in an aliphatic acyl radical, for example in an acetyl radical, or in the ß-position or in a- and ß-positions of a propionyl or ß-position, are also suitable as reactive dyes Acroyl radical, which is suitably bound to an amino group of the dye molecule, or in a heterocyclic radical, for example in a pyrimidine, pyridazine, quinoxaline, 2-halobenzothiazole

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or triazine ring, which is directly or via a -CO- group is bound to an amino group of the dye molecule.

Particularly favorable results are achieved with those reactive dyes which differ from sulfonic acid groups derive containing azo dyes and as reactive groups at least one di- or trihalopyrimidine, Dihaloquinoxaline or mono- or dihalotriazinylamino radical contain.

Also dyes that only appear in the course of the dyeing process metallized can be used with success. So have ο, ο'-dihydroxy azo dyes or Dyes containing ο-hydroxy-o'-carboxy groups Proven to be suitable. Chromium (III) salts, dichromate or copper sulfate may be mentioned as metal-releasing agents. Dyes that are only dispersible in water, when finely ground and with the aid of dispersants, form watery ones Suspensions from which the dyes are absorbed onto the textile material. These dispersible dyes can be metal-free or contain metal bound in complexes. So-called metal-free disperse dyes are advantageously used for polyester material and metal complexed containing dispersed dyes for synthetic materials Polyamide.

The water-soluble acidic wool is particularly suitable for dyeing natural and synthetic polyamides.

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dyes belonging to the various classes mentioned belong, i.e. those whose coloring component is a Anion is. Metal-free, metallized azo dyes are preferred Azo dyes, which contain two molecules of azo dye bound to a metal atom, can be re-chromable Azo dyes and anthraquinone dyes.

The reactive dyes mentioned are suitable for dyeing both wool and cotton Substrates react and which differ especially from the azo, pormazan, anthraquinone or phthalocyanine dyes derive. For dyeing cellulose, especially cotton and other native or regenerated vegetable textile material, are the so-called nouns, possibly mono-, dis- or heavy metal containing Polyazo dyes, anthraquinone dyes, nitro or Phthalocyanine dyes are suitable, as are the azo dyes that can be metallized on the substrate, in particular copper ones.

For coloring synthetic materials such as polyesters, polyacrylonitriles and their copolymers dispersed azo, anthraquinone, nitro, methine, xanthene, naphthazarine and quinophthalone dyes that are free from Water-soluble groups are especially suitable. When dyeing polyester fibers or fiber materials containing them, it is advisable to add so-called color transfer agents to the dyebath (Carrier) to be added in order to obtain a perfect coloration.

For dyeing textile material made of polyacrylonitrile and its copolymers or of synthetic, acidic

Modified polyamide is preferably used basic dyes, that is, those whose coloring component is a cation, namely methine, azomethine, tri- and diphenylmethane dyes.

. As surface-active auxiliaries, which may be used in the aqueous impregnation liquor, Both nonionic and ionic, i.e. anionic and cationic compounds can be used.

Suitable representatives of such surface-active compounds belong to the following types of compounds: Ethers of polyhydroxy compounds, such as polyoxyalkylated fatty alcohols, polyoxyalkylated polyols, polyoxyalkylated Mercaptans and aliphatic amines, polyoxyalkylated alkylphenols and naphthols, polyoxyalkylated alkylaryl mercaptans and alkylarylamines, also the corresponding esters of these compounds with polybasic acids, such as Sulfuric or phosphoric acid, optionally also in the form of ammonium or amine salts, fatty acid esters of Ethylene and polyethylene glycols as well as propylene and butylene glycol, glycerol and sugar alcohols such as sorbitol, N-hydroxyalkyl-carbonamides, polyoxalkylated Carbonamides and sulfonamides.

Particular mention should be made of the reaction products of higher molecular weight fatty acids and hydroxyalkylamines and their ethylene oxide addition products. Let this

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205698

for example from fatty acids from about 8 to -20 Carbon atoms, e.g. caprylic acid, stearic acid, oleic acid and in particular the acid mixture summarized under the collective term coconut fatty acid, and hydroxyalkylamines such as triethanolamine or diethanolamine. The molecular ratio between hydroxyalkylamine and fatty acid is preferably greater than 1, e.g. 2: 1.

Also suitable are alkylene oxide, especially ethylene oxide condensation products of saturated and unsaturated fatty alcohols with 8 to 20 carbon atoms, of saturated fatty acids with 8 to 20 carbon atoms, of alkylphenols with one or more alkyl substituents which together have at least 8 carbon atoms, of primary or secondary, aliphatic and cycloaliphatic, amines containing a higher alkyl or alkenyl radical of at least 8 carbon atoms, or of alkanolamides, aminoalkylamides and aminoalkyl esters of higher aliphatic carboxylic acids.

Ethers should the number of alkenoxy groups in these polyglycol ether be so large that the compounds in water are at least readily dispersible and preferably soluble in, and is 2 to up to the 100th

Anionic auxiliaries are obtained when the mentioned nonionic auxiliaries are used with an organic

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African dicarboxylic acids such as maleic acid, malonic acid or succinic acid, but preferably with an inorganic polybasic acid such as phosphoric or especially sulfuric acid, converted into an acid ester. The corresponding alkali metal, ammonium or amine salts of these esters can also be used.

Cation-active auxiliaries are obtained, for example, by quaternizing nitrogen-containing polyethylene glycol ether derivatives.

All of the auxiliaries mentioned can be used individually or in a mixture with one another.

The quantitative proportion of auxiliaries in the impregnation liquor depends on the amount of dye and the substrate, but should not exceed 15 to 20 g th and is preferably 0.5 to 5 g / l.

If desired, the fleet also contains Thickener. One uses, for example, cellulose-based thickeners, such as locust bean gum, galactomannans, tragacanth, British gum or water-soluble salts of alginic acids. Also are methyl cellulose or soluble salts of carboxymethyl cellulose are suitable. It is important to ensure that the thickener result in no precipitation under the application conditions. Other additives that the dyeing Preparation may contain electrolytes such as salts

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- ίο -

and acids. Sodium sulphate, ammonium sulphate or sodium chloride are expediently used as salts and aliphatic mono- or dicarboxylic acids which, apart from the carboxy carbon atom, have a maximum of k carbon atoms in the aliphatic chain, but only formic and acetic acid are of practical importance. Sulfuric and phosphoric acids may also be mentioned of the inorganic acids which can also be used. The p "value range

ri

of the dyeing preparations depends on the substrate to be colored and the particular dyes used.

It is expedient to dye p "values of 4 to 8.

ri

Finally, the impregnating liquor that can be used can also be bactericidal and / or fungicidal, for example Compounds and protective substances against insect caused damage, namely moth repellants, and also compounds for softening, antistatic treatment or as a flame retardant finish.

The impregnation liquors which can be used according to the invention is advantageously prepared by mixing warm aqueous dye solutions or dispersions of suitable dye Concentration with the surface-active substances that may be added Aids, thickeners, electrolytes and other additives.

The textile material is impregnated continuously with the help of a paint applicator by not doing that

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pre-wetted substrate is coated, sprayed, padded or padded with the dye liquor, for example, or also immersed in the dye liquor. The impregnation process expediently takes place at temperatures from 20 to 100.degree. C., preferably from 0 to 100.degree. The liquor uptake of the substrate can be a multiple of the weight of the substrate and is approximately in the range from $ 80 to $ 400, preferably from 200 to 300 %.

The dye is fixed, ie the impregnated goods are finished, in an aqueous bath at temperatures of 70 to 140 ° C., preferably 80 to 100 ° C. For materials on polyester fiber material, the fixing at temperatures of over 100 ° C. is preferably carried out under pressure. If the temperature during the impregnation process is below the specified ranges, it is advisable to bring the substrate to the desired temperature _{in a steaming channel that connects the devices for applying the dye and the fixing bath 3.} In principle, the use of a steaming channel between the two treatment steps is always appropriate in order to prevent the substrate from cooling down.

The impregnated textile material is treated in the fixing bath, which is usually located in a reel vat, for 5 to 60 minutes, preferably 10 to 30 minutes, at bath temperatures as indicated. For this discounted

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Continuous treatment in the reel vat, it is necessary to connect the beginning of the part to the end of the textile pieces, for example to sew.

The fixer contains acids such as formic or acetic acid, salts such as sodium chloride, sodium acetate, sodium sulfate, monosodium phosphate or disodium phosphate, and possibly also small amounts of the impregnation liquor, the amount of dye in the fixer not exceeding 20%, preferably 10 % of the amount of dye in the impregnation liquor target. Wetting and finishing substances can also be added. In the fixer, the dye is partially peeled off and redeployed, resulting in a level and true coloration on the substrate. The partial removal (bleeding) of the dye into the fixer should be kept within low limits. By adhering to temperature and _pH value ranges, as well as the applied amount impregnating one can control the bleeding.

The present method is found to be advantageous when dyeing thicker, stiffer or otherwise heavy manageable materials such as nonwovens, felts and, in particular, materials suitable as floor coverings such as carpets, for example needle felt, needle pile, knitted and Woven carpets. All of these materials (pile fabrics) have a distinct third dimension (fabric thickness, e.g. the

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- 45.-.

Pile height), whereby the material a einhekfc lend or also can have different pile heights, e.g. for loop pile or velor carpets (cut pile) The thickness of the goods (third dimension) covers approximately a range from 3 to 50 mm and depends on the respective substrate addicted.

The product thickness of the vast majority of the substrates is between 8 and 15 mm.

During the entire impregnation and fixing treatment, the compared to other textlien Flat structures quite dimensionally stable structures led widely. There is no wrinkling and the uniform The direction of the pile is retained.

The advantage of the present dyeing process, a combination of an impregnation process (paint application unit) and a fixing process (reel vat with fixing bath) represents, compared to the exhaust process for the piece dyeing of textile materials with a pronounced third Dimension lies in the considerably shortened dyeing time and a correspondingly reduced energy requirement, which was previously necessary for heating the liquor in a dyeing process lasting several hours. Furthermore, it was not foreseeable that it would be possible according to the method of the invention, textile material from a considerable The height of the goods, as occurs with carpet materials, is to be dyed evenly in a short time and also the shorter treatment will cause fiber damage,

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e.g. the occurrence of matting or changes in the pile direction is avoided.

In the following examples, parts are parts by weight and percentages are percentages by weight. The temperatures are given in degrees Celsius. CJ. means Color Index., Second Edition 1956 * published by The Society of Dyers and Colourists, Bradford, England and The American Association of Textile Chemists and Colorists, Lowell, Mass. UNITED STATES.

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Example 1 .

1000 m of raw carpet (polyamide needle pile) on a poulard with 13OO liters a 90 C hot Fleet that '

3.9 kg of CJ. Acid Yellow 25

5.2 kg of CJ. Acid Orange 3

2.5 kg of CJ. Acid Blue 72

2.6 kg of a reaction product of 8 moles of ethylene

oxide at ί mol p-tert. Octylphenol and 3.9 kg acetic acid (80 # ig)

contains, impregnated. The plot is $ 110. Then you drive with the impregnated material

into a reel skid, Indians call themselves 90 C, aqueous fleet of 39,000 liters is located. This fleet

contains: 3 g / l acetic acid (80 # ig) 2 g / l sodium acetate

1 liter of the impregnation liquor mentioned above per, 1000 liters.

The carpet material is in treated with the fixer. It is then cooled and rinsed by adding cold water.

You get one. level> green-olive coloring excellent preservation of the plot,

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- i6 -

Example 2

8OO m of a tufted carpet with polyamide pile

different paraffin affinity (so-called differential dyeing nylon) are in a color applicator with 1,800 liters of a 95 ° C hot liquor, the 1.8 kg CJ. Disperse Blue 7

3.24 kg of CJ. Acid Brown 283

3.6 kg of a reaction product of 8 moles of ethylene

oxide to 1 mole of p-tert. Octylphenol and 3.6 kg of acetic acid (80 $ ig)

contains, impregnated. The fleet take-up is $ 250. The impregnated material is then placed in an aqueous liquor of 3OOOO liters at 95 C a (reel skid). This fleet contains:

2 g / l acetic acid (80 $ ig)
2 g / l sodium acetate.

The carpet material is treated in the fixing bath at 98 ° C. for 17 minutes. Then cold water is added cooled and rinsed.

A uniform turquoise-blue coloration is obtained next to gray-black differentiation.

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Example 3

8OO m of a wool carpet (cut pile fabric)

are splashed with 2.6K0 liters of a 90 C hot liquor, the

21.12 kg of the dye of the formula

OH

HO Eq

A N = N

Cl

Cr

10.56 kg of the dye of the formula

0 NH,

SO ₃ H

ELC CH ₂ NHCOC = CH ₂

0 NH-

Cl

H ₃ C

42.24 kg of the dye of the formula '

OH HO -N = N-

SO ₂ NHCH ₃ COOCH ₃

Cr

blue

blue

Gray

10982 A / 22

26.40 kg of a mixture

1 part of the reaction product of 1 mole of coconut fatty acid with 2 moles of diethylamine and

1 part of the ammonium salt of acid sulfur acid ester of the adduct of mole of ethylene oxide with 1 mole of p-tert. Nonylphey

and 21.12 kg of formic acid ($ 85) contains. The plot is $ 150.

The impregnated material is then placed in a 95 G hot, aqueous 32,000 liter liquor

which is located in a reel skid. This fleet contains:

4 g / l formic acid (85 $ ig)

1 liter of the above-mentioned impregnation liquor per 1000 liters.

The carpet material is treated in the fixing bath at 98 ° C. for 15 minutes. It is then cooled by running cold water and rinsed.

The result is a blue coloration with excellent preservation of the appearance of the goods.

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Example 4

1000 m of a coniferous pile carpet with pile material

Consists of 8o ^ viscose and $ 20 synthetic polyamide (Nylon 66) are on a foulard with 1250 liters one 95 ° C hot liquor, the 11.25 kg of the. Dyestuff of the formula

-Έ Ή

ΛΑ-Ν SOH SO ₃ H SO H SOH Ν— / YS

/ S / S / S / s / S

HO S SO E

0.125 kg of the dye of the formula

GH ₅ CO HN

ν κ

OH, ^Ν Ν = Ν ~ <> - SO-H

* OH I ^

H0 "S S0, H OCH,

3 3

0.088 kg of the dye of the formula

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SCLH

HO 2056984 ά VN = N-
y AvAv blue HO S
SO ₃ H ^ χ A ^
NH ₂

2.5 kg of the ammonium salt of the acid sulfuric acid ester of the adduct of 2 moles of ethylene oxide with 1 mole of p-tert. Nonylphenol and

3 * contains 75 kg disodium phosphate, impregnated.

The fleet pickup is $ 120.

Then you drive with the impregnated material

into a reel skid, in which a 95 C is called, aqueous liquor of 29,000 liters is located. This fleet

contains: "

3 g / l disodium phosphate 15 g / l sodium chloride.

The carpet material is in treated with the fixer. It is then cooled and rinsed by adding cold water.

A uniform golden yellow color is obtained with good preservation of the appearance of the goods.

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Example 5 '

8θΟ m of a needle pile carpet with a polyamide pile of different heights (high-low pile) are sprayed with 720 liters of a 40 ° C warm liquor, the 15.12 kg .CJ. Acid Brown 248
0.144 kg CJ. Acid Red 57
0.3β0 kg CJ. Acid Blue 72
0.720 kg of a reaction product of 8 mol

Ethylene oxide on 1 mole of p-tert-octyl- ■ \

phenol,

1.440 kg of acetic acid (80%) and 1.440 kg starch ether thickening (solvitosis)

contains.

The plot size is 95 #.

The impregnated material is then driven through a steaming channel 2 m long into a liquor of 30,000 liters

at a temperature of 95 C (reel skid). The liquor contains 2 g / l acetic acid (80%). The carpet material * is treated in the fixing bath at 98 ° C. for 12 minutes. It is then cooled and rinsed by adding cold water. The result is a uniform beige coloration with excellent preservation of the fabric appearance and good pile development.

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Example 6

200 m raw carpet in 4 m width with polyacrylonitrile pile On a jute backing material, there is a 1,800 liter capacity across the entire width on the plank side 90 ° C hot dye liquor of the following composition evenly poured:

1.2 g / L CJ. Basic Blue 4l
0.3 g / l CJ. Basic Red 60
1.0 g / l acetic acid (80 $ ig)

The plot pick-up is 200 %, based on the weight of the carpet.

The impregnated material is then dyed in a 90 C hot, watery liquor of 28,000 liters a (reel skid). This liquor contains 1 g / l sodium acetate (crystalline) and 1 g / l acetic acid (80%). The carpet material is treated for 25 minutes at 98 ° G in the fixer, then it is cooled and rinsed by adding cold water. A uniform light violet coloration is obtained.

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Example 7

18O m of a tufted carpet 450 cm wide with pile material made from a yarn mixture containing 70 % nylon and 3 % polyester are impregnated in a parb applicator with 2800 liters of a 95 C hot liquor

1.1 kg of CJ. Disperse Yellow 42 g

1.8 kg CJ. Direct Yellow 12 '

0.4 kg of CJ. Acid Blue 80 and

5.6 kg acetic acid ($ 80)

contains. The liquor pick-up is 3OO %.

The mixture is subsequently stained with the thus-impregnated material in a 98 ⁰ C hot aqueous liquor of a 3OOOO liters (winch). This fleet contains

1 g / l acetic acid (80 # ig)
Ii5 g / l orthorphenylphenol
1 l / lOOO 1 of the above-mentioned impregnation liquor.

Treat the carpet material for 30 minutes 98 ° C in the fixer. It is then cooled and rinsed by adding cold water.

A level two-tone dyeing is obtained in the colors yellow and green.

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Claims (24)

Claims ti.) Process for dyeing organic, wide-spread textile material with a pronounced third dimension, characterized in that the textile material is subjected to a treatment which essentially consists of a) Impregnation of the material with an aqueous dye liquor containing a fiber-affine dye and optionally a surface-active aid contains, and b) treating the impregnated material in an aqueous bath during one for fixation sufficient period of time for the dye, and then finished by rinsing and drying. 2. The method according to claim 1, characterized in that one a) the textile material with an aqueous dye liquor containing a fiber-affine dye and optionally contains a surface-active dyeing auxiliary, continuously impregnated and b) intermittently in an aqueous bath for a time sufficient for fixation fixed. 3 · Method according to one of claims 1 and 2, characterized characterized in that the textile material with a 109824/2234 Dye-resistant preparation, the p _u value range of which is between 4 and 8, continuously impregnated at temperatures between 40 and 100 ° C. up to a liquor pick-up of 80 to 400 ° C. and then for 5 to 60 minutes at temperatures of 70 to 140. C fixes the applied dye in an aqueous bath. 4. The method according to claim 3 *, characterized in that that you impregnate carpets made of organic fiber material at temperatures of 40 to 100 C and then ^ send for 5 to 60 minutes at temperatures from 70 to 140 ° C fixed the applied dye in an aqueous bath. 5. The method according to claim 1, characterized in that that one as surface-active auxiliaries in the impregnation liquor reaction products of ethylene oxide long-chain alcohols with 8 to 20 carbon atoms, on alkylphenols with at least 8 carbon atoms send alkyl substituents or their esters of polybasic acids used. 6. The method according to claim 1, characterized in that as surface-active auxiliaries in the Impregnation liquor conversion products of higher molecular weight Fatty acids with 8 to 20 carbon atoms and hydroxyalkyl lines used. ■ 109824/2 234 7. The method according to claim 4, characterized in that one wide-guided carpet material at 90 to
100 ° C impregnated. 8. The method according to claim 4, characterized in that the impregnation liquor is applied to the carpet material pours on, patted up, sprayed on or the carpet material padded or immersed in the fleet. 9. The method according to claim 4, characterized in that that the impregnated carpet material is brought to the temperature of the fixing bath in a heating stage 10. The method according to claim 4, characterized in that one fixes at temperatures of 70 to 100 C. 11. The method according to claim 4, characterized in that polyester carpets at temperatures up to
Treated 140 ° C under pressure in a fixer. 12. The method according to claim 4, characterized in that the carpet material for 10 to 30 minutes in
Fixer treated. 13. The method according to claim 4, characterized in that the fixing bath acids, salts and optionally
Contains small amounts of the impregnation liquor. 109824/2234 14. The method according to claim I3, characterized in that that the fixer contains formic acid or acetic acid. 15 · The method according to claim 4, characterized in that needle felt, tufted, knitted and woven carpets dyes from organic fiber material. 16. The method according to claim 15, characterized in that that you dye wool carpets. 17 · The method according to claim 15 * characterized in that that you dye carpets made of synthetic polyamide fiber material. 18. The method according to claim 17 *, characterized in that carpets made of synthetic polyamide fiber material dyes with different dye affinity (differential dyeing). 19. Process part according to claim I5, characterized in that that you dye carpets made of polyester fibers. ™ 20. The method according to claim I5, characterized in that that carpets made of polyacrylonitrile fibers are dyed, 21. · The method according to claim 15, characterized in that carpets made of mixed organic fibers are dyed. 22. The method according to claim 21, characterized in that that carpets made of wool-polyacrylonitrile fiber colors. 109824/2234 23 · The method according to claim 21, characterized in that that one rugs made of synthetic polyamide-viscose fiber blends colors. 24. The method according to any one of claims 15 to 23, characterized characterized in that carpet material is dyed with a uniform or different pile height. 109824/2234