DE1965765A1 - Process for washing freshly dyed textile material - Google Patents

Description

CIBA AKTIENGESELLSCHAFT, BASEL (SWITZERLAND)

Case 6642 / E
Germany

Process for washing freshly dyed textile material.

Various proposals have been made to use textile materials, • especially textile materials based on synthetic fibers, to dye in baths with organic liquors, the process being carried out either continuously or discontinuously. In all of these processes, however, it is suggested that the textile material, if anything, wash in aqueous medium. This transition from the organic to the aqueous phase requires however, two thorough drying and large equipment Effort that becomes even greater when the textile material is subsequently used the dyeing process is subjected to a finishing treatment in the organic phase, such as hydrophobization or flame retardant finish in a solvent bath.

T216

BATH ORIGINAL

The present invention relates to a method for washing fresh from organic medium colored fiber material, which is characterized in that the fiber material is in a chlorinated aliphatic Hydrocarbon, which optionally is a surfactant and / or a dipolar, aprotic solvent contains, moved with the addition of heat and the organic solvent is then removed.

As substrates, textile materials made of synthetic fibers come into question, such as acrylic or Acrylonitrile fibers, polyacrylonitrile fibers and mixed polymers of acrylonitrile and other vinyl compounds, such as acrylic esters, Acrylamides, vinyl pyridine, vinyl chloride or vinylidene chloride, copolymers of dicyanethylene and vinyl acetate, as well as from acrylonitrile block copolymers, fibers made from polyurethanes, metal-modified or base-modified Polyolefins, especially polypropylenes, cellulose tri- and 2 l / 2-acetate and especially fibers made of polyamides, such as nylon-6, nylon-6,6 or nylon 12 made from aromatic polyesters, such as those made from terephthalic acid and ethylene glycol or 1,4-dimethylcyclohexane, and copolymers made from terephthalic and isophthalic acid and ethylene glycol or natural fibers such as wool, silk or cotton, as well regenerate cellulose materials.

00983a / 1216 BATH ORIGINAL

As a solvent, which is largely inert towards the fibers or filaments even at dyeing temperatures must be, i.e. they must not dissolve, halogenated aliphatic hydrocarbons such as carbon tetrachloride are used, Chloroform, methylene chloride, trichlorethylene, tetrachloroethane, dibromoethylene and especially perchlorethylene or trichlorethylene.

The chlorinated hydrocarbons can also use a polar, aprotic solvent, such as N, N-dimethylformamide, NN-dimethylacetamide, bis- 'dimethylnmido) methane phosphate, tris-'dimethylamido) phosphate, N-methylpyrrolidon, 1,5-rimethylpyrrolidone, NN- Dimethyl methoxyacetamide, NN, N ¹ , N'-tetramethylurea, tetramethylene sulfone (sulfolane), 3-methylsulfolane or dimethyl sulfoxide.

To avoid fiber damage;: u, one will be in usually more than 50 $ of the chlorinated aliphatic hydrocarbon to add.

Preferred mixtures contain e.g. 2 to) 0 Weight-f of a 3pretischen solvent and 98 to 70 Weight - ^ of a chlorinated, preferably aliphatic, hydrocarbon.

0098 3 0/1216

BAD OFIIGiNAL

The present process is preferably carried out without the addition of dispersants. This results in the advantage of easier drying of the washed textile material by evaporation of the solvent. Optionally, however, surfactants can also be added to the wash liquor. especially as additives to hydrophobic solvents with relatively little aunflöcungsbarkeit.

Important representatives of such surfactants include in particular to the following non-ionic compound types:

a) Polyglycol compounds, such as polyoxalkylated fatty alcohols, polyoxalkylated polyols, polyoxalkylated Mercaptans and aliphatic amines, polyoxyalkylated alkylphenols and naphthols, polyoxyalkylated alkylaryl mercaptans and alkylarylamines.

b) fatty acid esters of ethylene and polyethylene glycols, as well as propylene and eutylene glycol, glycerine or the polyrlycerols and pentaerythritol, as well as of sugar alcohols such as sorbitol, sorbitans and sucrose.

c) N-hydroxyalkyl carbonamides, polyoxyalkylated carbonamides and sulfonamides.

d) Liquid polyalkylene glycols, especially polyethylene glycols.

00 98 30/1216 BAD ORiGJNAl.

For example, surfactants from these groups which can be used advantageously may be mentioned: addition products of 8 moles of ethylene oxide with 1 mole of p-tert.-octylphenol, of 15 or 6 moles of ethylene oxide with castor oil, of 20 moles of ethylene oxide with the alcohol C, gH OH, ethylene oxide Adducts of di- [a-phenylethyl] phenols, polyethylene oxide tert-dodecylthioether, polyamine, polyglycol ethers or adducts of 15 or 50 moles of ethylene oxide with 1 mole of amine C ₁₉ H ₃ NH ₂ or C ₁₃ II NH ₃ .

Particularly valuable surfactants are sodium sulfosuccinate, Sodium alkylarylsulfonates, amine alkylarylsulfonates, Fatty acid esters of sorbitan, ethoxylated alkanolamides, ethoxylated phenols and ethoxylated phosphate esters. the Surfactants advantageously have FI.L.B. values of 5 to 8. The The definition of the H.L.B. values can be found in the work "interfacial Phenomena" by J.T. Davies and E.K. Rideal, New York, 19β5> P. 571 to 575

When washing out, the textile material to be dyed can be in the form of loose material, fleece, yarn or as a knitted fabric or tissue are present. It is available in loose form or in a form applied to a mechanical device in one stationary bath, especially in suitable jiggers, reel runners or cross reel dyeing machines, depending on the nature

009830/121 6

BATH ORIGINAL

the goods to be dyed, but especially in drum washing machines, washed, whereby V / arme must be added. Advantageously, the temperature is the wash liquor ¹ IO to 130 ° C.

Washing out can take place in apparatus or vessels that are in contact with the outside atmosphere (if necessary through a reflux condenser) * or in closed vessels, such as pressure vessels, with or without pressure.

After washing out, the dyed goods are taken out of the solvent bath and removed of the still adhering solvent either with steam

or treated with a stream of hot air. ■ - I

In the following examples, unless stated otherwise, the parts are parts by weight, the percentages are percentages by weight and the temperatures are given in degrees Celsius.

009830/1216

BATH ORIGINAL Example 1.

0.1 part of the dye!, P
3,7-dibromo-anthraquinone was dissolved in perchlorethylene at boiling point and the solution was then cooled to about 100%. 2.5 parts of non-pretreated textured polyester tricot knitted fabric (Crimplene) were added to the solution and at a liquor ratio of 1:64 in 100 parts of perchlorethylene for 45 minutes at boiling temperature (121.2) in a kettle equipped with a reflux condenser with recovery of the evaporating solvent colored. It was then cooled for 15 minutes and the dyed yarn was freed from the dye liquor adhering to it by centrifugation. The non-fixed dye adhering to the surface was then removed by an aftertreatment for 5 minutes at 50-60 in perchlorethylene, without intermediate drying, in order to achieve the desired brilliant shade and the maximum fastness properties. It was then centrifuged and dried in a stream of warm air.

The effect achieved with this aftertreatment (purity of shade, fastness properties) corresponds to that of the same coloration, after the dyeing with a blind vat consisting of 5 ml / 1 NaOH 1On and 2 g / l hydrosulfite by a treatment can be achieved from aqueous solution for 50 minutes at 60 °.

0098 30/1216

BATH ORIGINAL Example 2.

A red dye made using the exhaust dyeing process

on nylon-6-tufting-Tepplch (Perlon) with the dye of Formql

Cl
Gl-CII-CH -NHSO ₀ - <> —N = N- < > —N (CII _O CH _? QH)

d. ei d / c dd

CH

was then freed on the dyeing by centrifugation of the ψ adhering dye liquor. The non-fixed dye adhering to the surface was then, without prior intermediate drying, to achieve the desired brilliant shade and the maximum fastness properties, by rinsing the surface with cold rinsing with perchlorethylene for 5 minutes and then treating for about 10 minutes at 40-50 with a perchlorethylene liquor, polygamy 2 g / l polyethylene glycol (j500) oleic acid ester is removed.

This treatment was followed by a short rinse with cold perchlorethylene, then the goods were centrifuged and dried. The effect achieved with this aftertreatment corresponds to that of the same coloration achieved with a conventional detergent made from hot aqueous liquor.

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BAO ORIGINAL

example J>.

2 parts of the dye of the formula

HC — rN — CH, N C — N = N-

ZnCl.

CH

in the form of the concentrated dye powder were at boiling temperature in a solvent mixture consisting of 95 parts of perchlorethylene and 5 parts of dimethylacetamide dissolved, then the solution cooled to about 100.

100 parts dry, untreated polyacrylonitrile tricot fabric (Orion high bulk) was added and at a liquor ratio of 1:40 for 45 minutes at the boiling temperature (121) in a flask equipped with a reflux condenser with recovery of the evaporating solvent (according to the distillation reflux principle) with the addition of 1 part of the product of the formula

CIL

CH.

N-CH ₀ CH-CHCH ₀ -NC _{1 O}

CH.

OH OH

CH.

Anion "

colored. It was then cooled for 15 minutes and that dyed knitted fabrics freed from the dye liquor adhering to them by centrifugation.

It was then achieved without prior drying the desired brilliant shade and the maximum fastness properties of the non-fixed dye adhering to the surface by briefly

009830/1216

BATH ORIGINAL

- ίο -

Rinse with cold Perchioräthylon, which 10; i Whore thy lace tamid contains, and subsequent treatment in the same solvent mixture however, with the addition of 2 g / l of the kelsic acid ester of polyethylene glycol 300 at 40, it was removed for about 10 minutes. The stain was then centrifuged and dried directly after draining the bath.

This aftertreatment achieves the same effect that can be achieved if the dyeing is done by hot treatment. . act in water with 2 g / l of an adduct of 1 mole of nonylphenol and 9 moles of ethylene oxide after-cleaned.

009830/1216

BATH ORIGINAL Example 4.

0.32 g of the dye of the formula

Eq

_{N = N.}

■ Nil-C G-NH-A-CH =

are dissolved in 10 parts by volume of hot water. The solution is cooled and calcined soda is added to a concentration of 10 g / l. The dye solution obtained is mixed with 90 parts by volume of perchlorethylene which contains 20 g / l of an oleic acid ethylene oxide adduct (average molecular weight 300). 10 parts of dry, non-pretreated mercerized cotton yarn are added to the emulsion prepared in this way. (Density of the liquor = l, 6l 10 parts yarn in 200 parts by volume liquor) is after heating while ^l j h minutes at boiling temperature in an open system with recovery of vaporized solvent by a reflux condenser at a liquor ratio of 1:32 colored without further additives. Following dyeing, the cotton yarn was freed from the dye liquor adhering to it by centrifugation.

It was then, without intermediate drying, to achieve the desired brilliant shade and the maximum fastness properties non-reactively fixed dye by brief cold rinsing with perehlorethylene and subsequent treatment for about 10 minutes 50-60 ° with a rerchloräthylen / water emulsion (9: 1), which

rat Ii ν ) 098

30/1216

BATH ORIGINAL

- 32 ~

10 g / l of the oleic acid ester of polyethylene glycol (molecular weight 300) contains, removed. Subsequent to your treatment was again rinsed briefly with cold perchlorethylene, then centrifuged the vars and dried.

The effect achieved with this post-wash corresponds to that of a customary post-treatment from boiling water Liquor, with the addition of synthetic detergents or soap.

009830/12 16

BATH ORIGINAL

Example 5

Polyester filament fabric (terylene twill) was made with a solution of 20 parts of the dye of the formula

C _n IL CN

N
^N C II OCOCII

Cold padded in 1000 parts of a mixture of 10% perchlorethylene and 10 $ dimethylacetamide, squeezed off to 34 $ of the fiber weight, dried at 40-50 in a stream of warm air and then heat-set for 60 seconds at 210. The fabric was then treated by continuous treatment on a Breit after-treatment unit, first in a cold perchlorethylene / dimethylacetamide mixture (9 ^; l) (2 passages) and subsequent warm treatment at 40-50 °

, with 2 g / l des /
/ Oleic acid ester of polyethylene glycol ^ 00 (1-3 passages) in the same solvent mixture, as well as cleaned by a short cold rinse at the end '(1-2 passages) with pure porchlorethylene. The goods were then squeezed off like a pad and then dried. This aftertreatment from solvent gives a brilliant red coloration that is fast to rubbing.

009830/1216

BATH ORIGINAL

Bo! Game 6.

Nylon 6, β fabric is mixed with a solution of 10 parts of the Dye of the formula

_C1 / \ _N / \ _NH

CH

1000 parts of a mixture of 90 $ perchlorethylene and 10 $ di- ■ ™ methylacetamide padded cold, squeezed off to ^ 2% of the fiber weight., Dried at 40-50 in a stream of warm air and then heat-set at 200 for one minute. The fabric was subsequently treated by continuous treatment on a Breit post-treatment unit by initially cold rinsing (1-2 passages) with pure perchlorethylene, then passing through 1-5 warm. .

of 50 ° / · perchlorethylene baths / which contains 5 g / l detergent booster

and brief rinsing with cold perchlorethylene (1 passage).

As a result of this subsequent cleaning from solvent, the non-reactively bound dye is detached from the fiber and is obtained such a brilliant rub- and wet-fast yellow color.

0 09830/1216

BATH ORIGINAL

_ ₁₅ _ Ί965765

Example 7.

Polyacrylonitrile pile fabric (Orion) is mixed with a solution of 10 parts of the dye of the formula

0 NHCIL

0 NH (CH2) 3 -N (CH ₅₎ 2
Cold padded in 1000 parts of ferchlorethylene and squeezed off to 106% of the fiber weight. The fabric is dried and then heat-set for 90 seconds at 200 °. The fabric was then heat-set by continuous treatment on a Breit after-treatment unit by brief rinsing (1 pass! In perchlorethylene at 60 and then passing through 1-2 baths of cold perchlorethylene, which contains 2 g / l of the oil acid ester of polyethylene glycol 200 , as well as a short post

at 40 ° / rinse (1 passage) with warm perchlorethylene / post-cleaned. As a result of the subsequent solvent cleaning used, a blue dyeing that is more level and rubbing-fast is obtained compared to the dyeing that has not been cleaned up.

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BATH ORIGINAL

Example 8.

One in the continuous dyeing process according to the thermosetting method (2 cold pad passages, dry 1 minute at 100 °, heat set for 2 minutes at 1 ^ 0 °) with 10 g / l of the dye of the formula

Cl CH Ν ^{κ 3}

OCH

-N = N- < y -ν "° ^H 3

and pure perchlorethylene as a solvent on unmodified Dyeing produced from polypropylene fabric was then heat-set, by continuous treatment on a Breit aftertreatment system by rinsing with perchlorethylene at 60 °

(l passage) and subsequent washing out with warm perchloric egg ¹ JO /
ethylene / which 2 g / l of the oleic acid ester of polyethylene glycol ^ 00

contains, post-cleaned.

At the end there was another passage of cold perchlor- ' Ethylene rinsed, squeezed and dried.

Due to the applied solvent machine cleaning, im Compared to the non-aftertreated dyeing, a purer dyeing that is more resistant to rubbing is obtained.

009830/1216

Example 9

Bleached woolen fabric was made with a cold solution (10 g / l) of the dye of the formula

OH

ClCH CONH- <> -N = N-in a mixture of perchlorethylene: dimethyl acetamide (9 "l) in. padded two passages, dried at 100 ° for 1 minute and heat-set at 200 ° for 1 minute. The dyed wool fabric was then to the heat setting by continuous treatment at boiling temperature on a wide post-treatment system (2-4 Passages) with perchlorethylene, which contains 5 g / l of an adduct of 0 ctadecyl alcohol and 55 mol of ethylene oxide, cleaned afterwards. Subsequent to this solvent post-purification, rinsing was carried out with cold perchlorethylene for 1 passage, squeezed and dried.

A brilliant and true yellow coloration was obtained. The shade and the fastness properties of this dyeing correspond to those which are otherwise obtained by normal aqueous hot rewash with the addition of synthetic detergents.

009830/121 6

BATH ORIGINAL

Claims (1)

Claims. ! ·· ⁼ Process for rewashing fiber material freshly dyed from an organic medium, characterized in that the fiber material is moved in a chlorinated aliphatic hydrocarbon, which optionally contains a surfactant and / or a polar, aprotic solvent, with the addition of heat, and the organic Solvent then removed. P 2. The method according to claim 1, characterized in that that only fully synthetic fibers produced by polymerization or polycondensation are used. j5. Method according to claim 1, characterized in that that at least partially made of natural fibers textiles are used. 4. The method according to claim J5, characterized in that that one uses textile materials made of wool. 5. The method according to claim J5, characterized., that one uses textile materials made of cotton. 6. The method according to claim J>, characterized in that mixed fabrics of natural and synthetic fibers are used. 7. The method according to claim 6, characterized in that that one cotton-polyester, wool-polyester or wool-polyamide fabric washes. 8. The method according to claims 1 to ¹ J, characterized in that the tissue is freed from excess solvent by centrifugation. 0 09830/1216 'S, BATH ORIGINAL 9. Process ger.äss claims 1 cis S, dac-urch characterized in that one is an aliphatic chlorinated hydrocarbon alone or in conjunction with a surfactant and / or one suitable for dissolving unstretched polyacrylonitrile Freed solvent. 10. The method according to claim 9, characterized in that an amide of a fatty acid is used as an additional solvent. 11. The method according to claim 9> characterized in that that a phosphoric acid amide, in particular phosphoric acid tris (dimethylamide), is used. 12. The method according to claim 1, characterized in that the laundry in connection with a continuous dyeing process and also carries out continuously. 15. Modification of the method according to claim 12, characterized characterized in that an emulsion of a chlorinated aliphatic hydrocarbon and water is used. ] A. . The washed obtained according to claims 1 to 5 Material. 009830/1216 BATH ORIGINAL