DE1003690B - Process for dyeing wool with complex heavy metal compounds of monoazo or azomethine dyes - Google Patents

Description

The invention relates to a dyeing process for wool, which is optionally mixed with other textile fibers, especially with wool-like synthetic polypeptide fibers, according to the new, time and energy-saving method with complex heavy metal compounds of monoazo and azomethine dyes that do not contain acidic, contain water-solubilizing groups, can be colored very evenly.

It is known that the complex heavy metal compounds of monoazo and azomethine dyes of the type 2 dye molecules with 1 atom of heavy metal, which do not contain any acidic, water-solubilizing groups, suitable for real dyeing of wool and wool-like fibers. They show in an aqueous dye liquor especially at higher temperatures of 70 to 90 °, a very pronounced affinity for natural and artificial Polypeptide fibers. This is usually so large that if you run through the critical one carelessly quickly Temperature range from 70 to 85 ° during dyeing with very rapid exhaustion of the baths and depending on the composition of the dyes in question is more or less pronounced and very uneven Coloring occurs. Such uneven colorations can also be achieved by long boiling Due to the low wandering capacity of these metal-containing dyes, they can no longer be corrected and are practical unusable.

The more recent literature therefore recommends using the pre-wetted dyeing method for this class of dyes Dyed goods in the usual additives such as Glauber's salt, ammonium sulfate or ammonium acetate and / or if necessary a weak acid prepared dye liquor to enter at 40 to 60 °, then slowly and carefully to boil and then cook for some time. By scrupulously monitoring the The temperature of the dyebath succeeds in controlling the absorption rate of the metal-containing dyes in such a way that that satisfactorily level dyeings are produced. On the other hand, experts expressly advise against to go into boiling baths with the dyed material (cf. J. G. Grundy, "The Dyer and Textile Printer", 1952, Vol. CVIII, No. 10, p. 685).

For an ongoing production, however, is a dyeing method with heavy losses in time, material and Energy connected, which is used either for working on fresh baths or for cooling down Forcing baths and putting such a wide temperature range under scrupulous supervision.

It has now been found that wool can optionally be mixed with other wool, especially wool-like ones Textile fibers, even at temperatures of 80 and more degrees Celsius, directly with complex heavy metal compounds of monoazo and azomethine dyes of type 2 dye molecules to 1 atom of heavy metal, the

Method of dyeing wool with

complex heavy metal compounds

of monoazo or azomethine dyes

Applicant:
JR Geigy A.-G., Basel (Switzerland)

Representative: Dr.-Ing. Dr. jur. H. Mediger, patent attorney, Munich 9, Aggensteinstr. 13th

Claimed priority:
Switzerland from March 6, 1953

Dr. Hans-Rud. Hirsbrunner, Basel (Switzerland),
has been named as the inventor

no acidic water-solubilizing groups, very uniform and color completely in a much shorter time, when starting the coloration of the appropriate pre-crosslinked and buffered material to be dyed in hot dye liquor from the p _H value of at least 7.5, and under vigorous circulation of the fleet or movement of the goods case of a reduced _pH value, the dyeing at boiling temperature leads to an end. Succeeds completely uniform so depending on the depth of shade and on the type of dye used and the p _H -value lowering agent in the very short time of 10 to 30 minutes, to produce fully developed dyeings of good fastness and penetration. As a further technical advantages are to be emphasized that no special supervision of dyeing is necessary and that the baths used for adjusting the volume and p _H -value without time- and energy-consuming cooling are immediately ready for use. In contrast to previously proposed methods, it is important the _pH value to adjust the liquor containing the product to be dyed prior to dyeing at least 7.5, and then let fall during dyeing, for example, 6.5. Advantageously, remains with the Ph "value is within those limits which preclude substantial wool damage, and selects for adjusting the p _H -value buffer mixtures of ammonium salts of inorganic or organic acids, for example ammonium sulfate or ammonium acetate and ammonia. An output p _H -value the liquor from 7.5 to 8.5 is recommended. the lowering of the p _H -value takes place in the open dyeing apparatus by the thermal

609 838 / 379-

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Dissociation of the ammonium salts and the volatility are 5 parts of ammonium sulfate and 1 part of ammonia (25%) of the ammonia. In the closed dyeing machine, too. At 90 °, the steam is turned off, introduced the hot liquor for this purpose slowly acidic substances, persistent circulated for purposes of compensation of the p _H -value, wherein an addition of partially or completely water soluble then after S minutes the _pH value to 7.8 set. Esters, which saponify during the dyeing process, are a 5 Now 0.2 parts of the complex chromium compound is a favorable measure. As the _pH value lowering agents of 4-chloro-2-aminophenol -> - 2-naphthol-6-sulfamide, are, for example, lower esters of aliphatic containing 2 dye molecules to 1 chromium atom, fed-oxyacids such as Äthyllactat or Diäthyltartrat, or give. The bathroom moves out relatively quickly; Here alkali salts of acidic half-esters of organic or quick boiling, and after 30 minutes of boiling, inorganic polybasic acids in question, for example the coloring is terminated; p _H 7.2 of the bath. Wise salts of alkyl sulfoacetates, sulfobers - a very uniform violet color, dialkyl steins, phthalic monoesters or never - are obtained

of the molecular fatty alcohol sulfonates. As further stained, and the whole block of material shows uniform rates are the dispersion, shade and strength customary in dyeing. Wetting agent permitted, if not necessary; at- 15 Beismel 2

for example, one can use the formaldehyde condensation

products of naphthalenesulfonic acids or the single-acting It is made according to the principle of dormant material and

kung products of ethylene oxide worked on higher fatty alcohols of the circulating liquor. Also use as a liquor container. a " packing machine " is used. The coils that are on

The 20 perforated sleeves that can be used in the process according to the invention are located in the liquor metal-containing Dyes are preferably complex, perforated spindles screwed into containers, which are used as Ma-Chrom- or cobalt compounds of o, o'-dioxy or material carriers are used. The circulation pump aro-carboxy-o'-oxyazo- or azomethine dyes, which are mutually, d. i.e., the fleet will be once from does not contain any acidic, water-solubilizing groups - pressed inside out and on the other hand from the outside th. Such substituents are sucked in here and below and through the sleeve and spindle to the pump referred to as acidic, water-solubilizing groups. The apparatus is locked. The Flotdie in neutral water with formation of a trihydroxotene ratio is 1:22.

dissociate nium ions, such as the carboxyl one loads the packing apparatus with 100 parts of wool

and the sulfonic acid group. Preferably, the worsted yarn and 2200 parts of soft water are conducted, the complex metal compounds usable according to the invention then operate the circulation pump and heat up. of such dyes from which sets the water during the heating to contain 2.5 parts compounds Ammonlöslichkeit favoring substituents, examples acetate, 1 part ammonia (25 ° / ₀ solution) and 5 parts Äthyllactat play sulfamide, organic or on nitrogen 5 Allocate diethyl tartrate. At 80 °, the vapor substituted sulfamide is disengaged from lower fatty acids, the hot liquor to the adjustment of the p _H -value derived acylamino or alkylsulfonyl groups. The dyeing method according to the invention is suitable for dyeing complex cobalt compound of 2-aminophenol-4-sulfof wool in all its processing stages, amide -> - /? - naphthol, containing 2 dye molecules, for example in the form of loose Material, yarn, felt on 1 cobalt atom added. It is dyed like in the Beiu. Like. Game 1 specified.

Even on dyeing machines that are operated at temperatures of 40. Very evenly through-dyed bobbins from Working 100 ° and more under pressure is the new mé wine red color, method applicable. Example 3

Also mixed fabrics, which are predominantly made of wool and

It is made on the principle of resting material and consists of other textile fibers, especially wool

and man-made polypeptide fibers, can be worked according to the 45 of the circulating liquor. You use one new method with the defined metal-containing dye - so-called strand dyeing apparatus as a liquor container. the dye fabrics perfectly. Yarns are hung on metal rails, which are in

The following examples serve to illustrate a metal support that is removably mounted. The beder Invention without limiting it. In it are the sent material carrier is one-parts into the liquor container, Unless otherwise noted, set as 50 weight and the liquor by means of a circulation pump parts understood and the temperatures in degrees Celsius pumped the apparatus. The liquor ratio is specified. Parts by weight are equivalent to parts by volume 1: 33.

such ratio as kilograms to liters. Working method: One prepares in the rope dyeing machine

Bath consisting of 3300 parts of soft water, 5 parts

Example 1 55 ammonium sulfate and 2 parts of ammonia (25 ° / ₀ ig), heated

to 80 ° and goes in with 100 parts of worsted wool

It is made on the principle of dormant material and strand shape. Work is carried out for 5 minutes at 80 ° in front of the circulating liquor. Left as a liquor container, the goods from the bath are then used as a " packing machine" ·. The charging of the apparatus, 1 part of the complex chromium compound, is carried out in such a way that winding bodies are screwed into perforated pipes in the liquor 60 4-nitro -2 - aminophenol - * - 3,4-dimethyl-1-phenol, which serve as a holding of 2 dye molecules on 1 chromium atom, added material carrier. The fleet is retracted and again with the goods. The dyeing by means of a circulation pump through the winding of is pressed in the usual way, as described in Example 1, inside out. The liquor ratio, carried out and completed, is 1:50. 65 Yarns of rust-brown color which are very evenly colored are obtained

How it works: 100 parts of wool are colored.

Shape of winding bodies in the packing apparatus as follows: "RpicnipT 4

colors: 5000 parts of soft water are allowed to flow in, .oeispiei <±

activates the circulation pump and heats with. In the packing apparatus according to example 1, individual felts are made

indirect steam. During heating, 70 sets stacked horizontally, making a package

arises, which can be fixed on the material carrier. Is colored according to the information and with the additives of Example 1 with a dye mixture, each consisting of 0.2 parts of the orange and red complex chromium compounds of 2-amino-phenol-4-sulfamide -y phenylmethyl-pyrazolone and 5-Nitramino-phenol -> - Phenyl-methyl-pyrazolone, containing 2 dye molecules on chromium.

Felt packets that are very evenly dyed through are obtained.

The following table contains further dyes which are after those described in the preceding examples Methods can be colored in an analogous way:

Tabel

complex chromium compound des

Dye containing 2 dye

molecules on 1 chromium atom

Azomethine dye from 2-aminophenol-4-sulfamide and 3, 5-dichloro-2-oxybenzaldehyde

Azo dye 2-aminophenol-4-methylsulphone -y acetoacetic -o-chloroanilide

Azo dye 2-aminophenol-4-ethylsulfone - * - Acetylamino-naphthol- (1.7)

Azo dye
ethylamide - * ■
(1.7)

2-aminophenol-4-sulf-acetylaminonaphthol-

Color of the wool dye

yellow

yellow

Gray

Gray

Claims (4)

Patent claims: 1. A method for dyeing wool, optionally mixed with other, especially wool-like, textile fibers with complex heavy metal compounds of monoazo or azomethine dyes of the type 2 dye molecules to 1 heavy metal atom that do not contain acidic, water-solubilizing groups, characterized in that the dyeing in hot dye liquor at a _pH value of at least 7, 5, after prior setting of dye bath and dyed fabric to this _pH-value, and the staining circulation of the fleet, or movement of the material begins at sedimenting _pH value at boiling heat to End leads. 2. The method of claim 1, characterized by the use of esters of low molecular weight alcohols which are hydrolyzed under the dyeing conditions, as the _pH value lowering agents. 3. The method according to claim 1, characterized by the use of ammonium salts, as the _pH value lowering agents. 4. The method according to claim 1, characterized by the use of a buffer mixture consisting of ammonium salts of inorganic or organic acids, and ammonia to adjust the initial p _H -value of the dyed fabric and the dye liquor. Considered publications:
German Patent No. 651 675;
British Patent No. 683,761;
U.S. Patent No. 2,520,080. © £ 09 838/379 2.