Classifications

• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
  • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
  • D06P1/673—Inorganic compounds
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
  • D06P3/02—Material containing basic nitrogen
  • D06P3/04—Material containing basic nitrogen containing amide groups
  • D06P3/06—Material containing basic nitrogen containing amide groups using acid dyes
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
  • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
  • D06P1/60—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
  • D06P1/607—Nitrogen-containing polyethers or their quaternary derivatives
  • D06P1/6076—Nitrogen-containing polyethers or their quaternary derivatives addition products of amines and alkylene oxides or oxiranes
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
  • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
  • D06P1/673—Inorganic compounds
  • D06P1/67333—Salts or hydroxides
  • D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
  • D06P3/02—Material containing basic nitrogen
  • D06P3/04—Material containing basic nitrogen containing amide groups
  • D06P3/14—Wool
  • D06P3/16—Wool using acid dyes
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
  • D06P3/02—Material containing basic nitrogen
  • D06P3/04—Material containing basic nitrogen containing amide groups
  • D06P3/24—Polyamides; Polyurethanes
  • D06P3/241—Polyamides; Polyurethanes using acid dyes
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S8/00—Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
  • Y10S8/916—Natural fiber dyeing
  • Y10S8/917—Wool or silk

Definitions

• the present invention relates to a new process for fiber and flat level dyeing of natural polyamide fiber materials with sulfo-containing 1: 1 metal complex dyes or with dye mixtures containing sulfo-containing 1: 1 metal complex dyes and metal-free sulfonic acid group-containing dyes from an aqueous liquor in the presence of 20 to 35 percent by weight of an alkali - And / or ammonium fluorosilicate, based on the amount by weight of the 1: 1 metal complex dye in the presence of an auxiliary, dyeing at a fiber-protecting pH of 3 to 5, the dye bath is practically completely stripped, the dye is well colored and good Overall fastness, in particular good wet fastness and good light fastness, as well as the material dyed by the new process and means for carrying out the process.
• a disadvantage of the dyeing processes used hitherto for natural or synthetic polyamide materials with 1: 1 metal complex dyes or mixtures of 1: 1 metal complex dyes with metal-free acid dyes is that these dyes or mixtures are dyed at a pH of approximately 1.9 to 2.8 must be in order to obtain level coloring.
• the pH value of the dyebath is of crucial importance in addition to the dyeing time, since natural and synthetic polyamide materials, especially wool, are strong both in the strongly acidic and in the alkaline pH range to be attacked.
• the present invention thus relates to a process for dyeing fiber material from natural polyamides from an aqueous liquor with dyes in the presence of alkali or ammonium salts and in the presence of auxiliaries, which is characterized in that these fiber materials are treated with at least one sulfo-containing 1: 1- Metal complex dye or with a mixture containing at least one sulfo group-containing 1: 1 metal complex dye and at least one sulfo group-containing metal-free dye in the presence of 20 to 35 percent by weight of an alkali and / or ammonium fluorosilicate, based on the amount by weight of the 1: 1 metal complex dye, in the presence of a Aids at pH 3 to 5 colors.
• the usable 1: 1 metal complex dyes containing sulfo groups are preferably monoazo or disazo dyes which contain a chromium ion as the metal ion.
• 1: 1 metal complex azomethine dyes, which preferably contain a chromium ion, can also be used.
• the usable sulfo-containing metal-free dyes are preferably acidic to strongly acidic acid dyes from the series of monoazo or polyazo, anthraquinone, triphenylmethane or xanthene dyes, which can contain the substituents customary for acid dyes.
• the sulfo-containing metal-free dyes can be substituted by fiber-reactive radicals.
• the amounts in which the defined dyes or dye mixtures are used in the dyebaths can vary within wide limits depending on the desired depth of color, in general amounts of from 0.01 to 10 percent by weight, based on the material to be dyed, of one or more dyes proven advantageous.
• Alkali or ammonium salts of hexafluorosilicic acid or mixtures thereof are used as alkali or ammonium fluorosilicates in the process according to the invention.
• Na2SiF6 or (NH4) 2SiF6 or a mixture of Na2SiF6 and (NH4) 2SiF6 is preferably used.
• the amount in which the alkali and / or ammonium fluorosilicate is used in the dye baths is 20 to 35 percent by weight, based on the amount by weight of the 1: 1 metal complex dye.
• amount by weight of the 1: 1 metal complex dye refers to the raw dye, i.e. to the amount by weight of a dye isolated by customary methods (e.g. salting out), which contains about 20 to 40 percent by weight of salt.
• auxiliaries which can be used in the process according to the invention are known per se and are produced by known methods. They are preferably leveling aids or mixtures of different leveling aids; anionic agents, cationic agents, nonionic agents and amphoteric agents or mixtures thereof can be considered.
• anionic agents substituted naphthalenesulfonic acids, sulfuric acid half-esters of ethoxylation products, salts of longer-chain alkanesulfonic acids, salts of alkylarylsulfonic acids, in particular dodecylbenzenesulfonic acids, fatty acid amide sulfonic acids, sulfuric acid half-esters of fatty amine polyglycol ethers.
• cationic agents are: Polyglycol ether of fatty amines, polyglycol ether of fatty acid amidamines, quaternary ammonium compounds.
• nonionic agents which may be mentioned are: polyglycol ethers of fatty alcohols, of alkylphenols, of resin acids, of fatty acid alkylolamides.
• amphoteric agents are: reaction products of ethoxylated fatty amines and hydroxyethanesulfonic acids, reaction products of phenol and styrene, polyethylene glycol difatty acid esters.
• Leveling aids containing compounds of the formula are preferably used wherein R is an alkyl or alkenyl radical having 12 to 22 carbon atoms, M is hydrogen, alkali metal or ammonium and m and n are integers, the sum of m and n being 2 to 14, or of the formula wherein R 'independently of R has the meaning given for R, A is an anion, Q is an optionally substituted alkyl radical and p and q are integers, the sum of p and q being 2 to 50, or of the formula wherein R "independently of R has the meaning given for R and x and y are integers, the sum of x and y being 80 to 140, a mixture containing compounds of the formula (1) and (2) or a mixture containing compounds of the formulas (1), (2) and (3) or a mixture comprising compounds of the formulas (1a), (2) and (3).
• leveling aid mixtures containing 5 to 70 parts by weight of the compound of the formula (1) or (1a), 15 to 60 part by weight of the compound of the formula (2) and 5 to 60 part by weight of the compound of the formula (3), based on 100, are used Parts by weight of the leveling agent mixture, where in the formulas (1), (1a), (2) and (3) R, R 'and R "independently of one another denote an alkyl or alkenyl radical having 16 to 22 carbon atoms.
• a and Q are derived from the quaternizing agents chloroacetamide, ethylene chlorohydrin, ethylene bromohydrin, epichlorohydrin, epibromohydrin or preferably dimethyl sulfate.
• a leveling aid mixture which, in addition to compounds of the formulas (1) or (1a), (2) and (3), where the sum of p and q in formula (2) is preferably 20 to 50 contains an adduct of 60 to 100 moles of ethylene oxide with one mole of C15-C20 alkenyl alcohol.
• a leveling agent mixture which contains the compounds of the formulas (1) and (2) or (1a) and (2), in which the sum of the symbols p and q in formula (2) is 4 to 10.
• a leveling aid mixture of compounds of the formula (2) in which the sum of the symbols p and q in formula (2) is 30 to 40 and R ⁇ is an alkyl radical having 15 to 22 carbon atoms.
• the very particularly preferred leveling aid mixture may contain, in addition to water, an adduct of 60 to 100 moles of ethylene oxide with one mole of C15-C20 alkenyl alcohol, preferably 80 moles of ethylene oxide with one mole of oleyl alcohol.
• the amount in which the leveling aid or the leveling aid mixture is used in the dyebaths can vary within wide limits, in general an amount of 0.3 to 3 percent by weight, preferably 1 to 2 percent by weight, based on the fiber material, of leveling aid or Leveling agent mixture proved to be advantageous.
• the dyebaths can contain mineral acids, such as sulfuric acid, sulfamic acid or phosphoric acid, organic acids, expediently lower, aliphatic carboxylic acids, such as formic, acetic or maleic acid.
• the acids primarily serve to adjust the pH of the liquors used according to the invention.
• the pH is preferably adjusted from 3 to 5 using an organic acid, in particular formic acid or acetic acid.
• the dye liquor of alkali or ammonium fluorosilicate can be various salts, in particular ammonium or alkali salts such as e.g. Contain ammonium sulfate or preferably sodium sulfate as an auxiliary. Preferably 1 to 10 percent by weight of ammonium or alkali salts, based on the fiber material, are used.
• the 1: 1 metal complex dyes which can be used in the process according to the invention are preferably those which have at least one 1: 1 chromium complex azo or azomethine dye with 1 to 3 sulfonic acid groups, in particular 1 to 2 sulfonic acid groups, and in the case of dye mixtures, at least one metal-free one Contain dye with 1 to 2 sulfonic acid groups.
• metal-free sulfo-containing dyes are used in the process according to the invention with good migration properties.
• the migrating ability of these dyes should correspond to the migrating ability of the 1: 1 chromium complex azo or azomethine dyes.
• the migratory capacity on wool is determined by treating a sample dyed to 1/1 standard depth together with an uncolored sample of the same weight in a blind bath.
• the treatment conditions for determining the migratory capacity correspond to the conditions given in Example 1 with regard to liquor ratio, pH and treatment duration.
• the evaluation is carried out by spectrophotometric determination of the amount of dye on the originally undyed wool as a percentage of the originally colored wool.
• a range of 25 to 50% has proven to be advantageous as good migratory power, colored at pH 4 to 5 and measured as a difference in strength.
• Suitable metal-free dyes containing sulfo groups are, for example, C.I. Acid Blue 1, 7, 13, 23, 40, 40: 1, 43, 45, 47, 72, 147, 258 and 277; C.I. Acid Red 1, 5, 37, 42, 52, 57 and 361; C.I. Acid Yellow 10, 17, 25, 27, 99 and 219; C.I. Acid Orange 1, 3 and 156; C.I. Acid Green 3, 9 and 16; C.I. Acid Violet 9 and 36; C.I. Acid Brown 10, 11 and 248.
• the color mixture of suitably selected yellow or understand orange, red and blue coloring dyes with which any desired shade of the visible color spectrum can be adjusted by a suitable choice of the proportions of the dyes.
• 1 chromium complex azo or azomethine dyes are those of the formula used, in which - (CO) 0 ⁇ 1-O- and (O or NR1) are bonded to D and K adjacent to the azo bridge, D the rest of a diazo component of the benzene or naphthalene series, K the rest of a coupling component of the benzene, Naphthalene or heterocyclic series or the acetoacetic acid arylide series, R1 hydrogen, or an optionally substituted alkyl or phenyl radical, M is a cation and An is an anion, and Y represents the nitrogen atom or the CH group.
• sulfo group-containing 1: 1 chromium complex azo or azomethine dyes of the formula (4) are preferably used, in which D is a benzene or naphthalene residue optionally substituted by halogen, C1-C--alkyl, C1-C4-alkoxy, nitro or sulfamoyl , K a optionally substituted by halogen, C1-C4-alkyl, C1-C4-alkoxy, C2-C4-alkanoyl-amino, sulfamoyl or hydroxy-phenyl-, naphthyl-, 1-phenyl-3-methylpyrazolone- (5) -, Acetoacetamide, especially acetoacetoanilide or quinoline, R1 is hydrogen and M is an alkali application.
• Y in formula (4) preferably denotes the nitrogen atom.
• the metal-free dyes containing sulfonic acid groups used in the process according to the invention are those of the dye series mentioned above which, for example, can be substituted by alkyl groups having 1 to 4 carbon atoms, such as methyl, ethyl, propyl, isopropyl and butyl, alkoxy groups having 1 to 4 carbon atoms, such as methoxy, ethoxy, propoxy, isopropoxy and butoxy, acylamino groups having 1 to 6 carbon atoms, such as acetylamino and Propionylamino, benzoylamino, amino, alkylamino with 1 to 4 carbon atoms, phenylamino, alkoxycarbonyl with 1 to 4 carbon atoms in the alkoxy radical, nitro, acetyl, cyano, trifluoromethyl, halogen, such as fluorine, chlorine and bromine, sulfamoyl, carbamoyl, ureido,
• the metal-free dyes containing sulfonic acid groups can be substituted by one or more fiber-reactive radicals.
• Suitable fiber-reactive radicals are, for example, the radicals mentioned in DE-OS 29 13 102.
• Mixtures of 1: 1 metal complex dyes containing sulfo groups and metal-free dyes containing sulfo groups are preferably used in the process according to the invention in a weight ratio of 40:60 to 95: 5.
• the sulfo-containing dyes used in the process according to the invention are present either in the form of their free sulfonic acid or preferably as their salts.
• suitable salts are the alkali, alkaline earth or ammonium salts or the salts of an organic amine.
• suitable salts include the sodium, lithium, potassium or ammonium salts or the salt of triethanolamine.
• the 1: 1 metal complex dyes containing sulfo groups used in the process according to the invention and the metal-free dyes containing sulfo groups are known per se and are obtained by known methods.
• the dye mixtures used in the process according to the invention can be prepared by mixing the individual dyes. This mixing process takes place, for example, in suitable mills, e.g. Ball or pin mills, as well as in kneaders or mixers.
• the dye mixtures can be prepared by spray drying the aqueous dye mixtures.
• the dyebaths can also contain other customary additives, such as Wool protection, wetting and defoaming agents included.
• the liquor ratio can be selected within a wide range, from 1: 6 to 1:80, preferably 1:10 to 1:30.
• Dyeing is carried out from an aqueous liquor using the exhaust process, e.g. at temperatures between 80 and 105 ° C or 110 ° C when using a formaldehyde-releasing wool protection agent, preferably between 98 and 103 ° C.
• the dyeing time is usually 30 to 120 minutes.
• the leveling aid and the alkali metal or ammonium fluorosilicate are expediently mixed into the aqueous dye liquor and applied simultaneously with the dye mixture.
• the fiber material is preferably added to a liquor which contains acid and auxiliaries and has a temperature of 30 to 70 ° C.
• the dye mixture and the alkali metal or ammonium fluorosilicate are then added and the temperature of the dyebath is increased at a rate of 0.75 to 3 ° C per Minute, optionally with a temperature stop during heating, in order to dye preferably in the specified temperature range from 80 ° C. to 105 ° C. for 30 to 120 minutes.
• the bath is cooled and the colored material rinsed and dried as usual.
• a particularly preferred procedure is characterized in that the fiber material is added to a liquor which contains acid and a leveling agent containing alkali and / or ammonium hexafluorosilicate and Na2SO4 and has a temperature of 30 to 70 ° C. Subsequently, the dyes or dye mixtures which contain alkali and / or ammonium hexafluorosilicate are added, and the temperature of the dyebath is increased at a heating rate of 0.75 to 3 ° C. per minute, optionally with a temperature stop during heating, in order to to color the specified temperature range from 80 ° C to 105 ° C. The bath is then cooled and the colored material rinsed and dried as usual.
• a textile fiber material made of natural polyamides which can be dyed according to the invention, above all wool, but also mixtures of wool / polyamide, wool / polyester, wool / cellulose or wool / polyacrylonitrile and silk should be mentioned.
• the fiber material can be in a wide variety of forms, e.g. as loose material, sliver, yarn and piece goods or as carpet.
• a particularly preferred embodiment of the process according to the invention is characterized in that natural polyamide fiber materials, in particular wool, with at least one dye mixture as defined above in the presence of ammonium fluorosilicate or sodium fluorosilicate in a 20 to 35% by weight amount, based on the weight amount of 1: 1 used Chromium complex dye, and in the presence of a leveling agent, containing compounds of the formula (1) and (2) or (1), (2) and (3) or (1a), (2) and (3), and in the presence of sodium sulfate colors at a pH of 3.7 to 4.2.
• the sulfo-containing, metal-free dyes used in the process according to the invention can contain one or more fiber-reactive groups.
• the sulfo-containing, metal-free dyes used in the process according to the invention can contain one or more fiber-reactive groups.
• Process uses such dye mixtures of the 1: 1 metal complex dyes defined according to the invention and the sulfo-containing metal-free dyes, in which the metal-free dyes used are either all reactive dyes or are all free from fiber-reactive groups; metal-free dyes containing sulfo groups are very particularly preferably used.
• a very particularly preferred embodiment of the method according to the invention is characterized in that the dye mixtures used according to the invention consist of such metal-containing and metal-free dyes defined according to the invention which give colorations of the same nuances, i.e. For example, the use of a mixture of at least one blue-coloring, 1: 1 metal complex dye containing sulfo groups and at least one blue-coloring, metal-free dye containing sulfo groups.
• the method according to the invention has the following advantages over the known methods for fiber material made from natural polyamides in addition to the already mentioned.
• the material dyed under the dyeing conditions mentioned has better overall fastness properties, in particular better wet fastness properties. Another important advantage is that the dyes are almost completely absorbed.
• the method according to the invention is preferably used for dyeing wool.
• the process according to the invention surprisingly manages with a significantly smaller amount of alkali metal or ammonium hexafluorosilicate.
• the invention further relates to a means for carrying out the method according to the invention.
• the agent is a solid mixture containing at least one 1: 1 metal complex dye containing sulfo groups, in particular a 1: 1 chromium complex dye, and if appropriate at least one sulfo-containing metal-free dye and 20 to 35 percent by weight of an alkali or ammonium fluorosilicate based on the 1: 1 metal complex weight amount.
• the mixture according to the invention is prepared by mixing at least one 1: 1 chromium complex dye containing sulfo groups and optionally at least one metal-free dye containing sulfo groups with 20 to 35 percent by weight (based on the weight of the 1: 1 metal complex dye) of alkali metal and / or ammonium fluorosilicate.
• the mixing process takes place, for example, in suitable mills, e.g. Ball or pin mills, as well as in kneaders or mixers.
• the solid mixtures can be used for dyeing natural textile polyamide fiber materials.
• Another means of carrying out the process according to the invention is a mixture comprising a leveling aid composed of one or more compounds of the formula (1), (1a), (2) or (3), in particular a leveling agent mixture composed of compounds of the formulas (1a), (2 ) and (3), and 5 to 25 weight percent alkali and / or ammonium hexafluorosilicate, preferably (NH4) 2SiF6, based on the amount by weight of the compounds of the formulas (1), (1a), (2) and / or (3).
• a leveling aid composed of one or more compounds of the formula (1), (1a), (2) or (3)
• a leveling agent mixture composed of compounds of the formulas (1a), (2 ) and (3)
• 5 to 25 weight percent alkali and / or ammonium hexafluorosilicate preferably (NH4) 2SiF6, based on the amount by weight of the compounds of the formulas (1), (1a), (2) and / or (3).
• the mixture is produced by mixing at least one compound of the formulas (1), (1a), (2) or (3) with 5 to 25 percent by weight of alkali and / or ammonium hexafluorosilicate.
• the mixing process takes place, for example, in suitable mixers.
• the mixture can be used together with the dye mixture containing alkali and / or ammonium hexafluorosilicate for dyeing natural polyamide fiber materials.
• the same preferences apply to the mixture as apply to the process.
• the following examples serve to illustrate the invention.
• the parts are parts by weight and the percentages are percentages by weight.
• the temperatures are given in degrees Celsius.
• the relationship between parts by weight and parts by volume is the same as that between grams and cubic centimeters.
• the indicated amounts of dye refer to raw dye.
• the dye liquor After adding a solution of 1.1 parts of the 1: 1 chromium complex of the dye of the formula 0.5 parts of the 1: 1 chromium complex of the dye of the formula 0.23 parts of the 1: 1 chromium complex of the dye of the formula 0.23 parts of the 1: 1 chromium complex of the dye of the formula 0.64 parts of the dye of the formula 0.97 parts of the dye of the formula and 0.4 parts of the dye of the formula the dye liquor is kept at 50 ° for a further 10 minutes and then heated to 98 ° at a heating rate of 0.8 ° / minute. The pH at the beginning of dyeing is 3.8. After 90 minutes at 98 °, the mixture is cooled to 50 ° and the dye liquor is drained off. The brown-colored wool yarn is rinsed at 50 ° for 10 minutes, then at room temperature and dried as usual. The medium brown color obtained is excellent in fiber and has good fastness properties.
• Example 2 100 parts of wool fabric are in a dyebath which contains 8 parts of sodium sulfate, 1.2 parts of the leveling aid given in Example 1 and 2.3 parts of 85% strength formic acid in 2000 parts of water at 40 ° for 15 minutes at 40 ° pretreated. The pH is 3.7.
• the dye liquor After adding a solution of 0.18 parts Na2SiF6 and 0.21 parts of the dye of the formula 0.26 parts of the dye of the formula 0.11 parts of the dye of the formula 0.11 parts of the dye of the formula 0.13 parts of the dye of the formula 0.11 parts of the dye of the formula and 0.12 parts of the dye of the formula the dye liquor is kept at 40 ° for a further 10 minutes and then heated to 70 ° at a rate of 1 ° per minute. After 20 minutes of dyeing at 70 °, the dye liquor is heated to 100 °. After 90 minutes of dyeing at 100 °, the mixture is cooled to 60 ° and the dye liquor is drained off. The brown-colored wool fabric is rinsed for 5 minutes at 50 °, then at room temperature and dried as usual. The dyeing obtained has excellent fiber shelf properties and good fastness properties.
• Example 3 100 parts of wool fabric are pretreated for 10 minutes at 40 ° in a dyebath which contains 1000 parts of water at 40 °, 8 parts of sodium sulfate, 1.5 parts of the leveling aid given in Example 1 and 2 parts of 85% formic acid .
• the pH is 3.8.
• After adding a solution containing 0.49 parts of the dye of the formula 0.13 parts of the dye of the formula and 0.12 parts (NH4) 2SiF6 the dye liquor is kept at 40 ° for a further 10 minutes and then heated to 100 ° at a heating rate of 0.8 ° per minute.
• the mixture is cooled to 60 ° and the dye liquor is drained off.
• the blue-colored wool fabric is rinsed and dried as usual.
• the medium blue color obtained is excellent fiber-level and has good fastness properties.
• Example 4 100 parts of wool fabric are in a dyebath which contains 8 parts of sodium sulfate, 1.2 parts of the leveling aid given in Example 1 and 2.3 parts of 85% formic acid for 40 minutes at 40 ° in 2000 parts of water at 40 ° pretreated. The pH is 3.7.
• the dyeing obtained has excellent fiber shelf properties and good fastness properties.
• the dye liquor After adding a 50 ° warm solution of 2.11 parts of the 1: 1 chromium complex of the dye of the formula 2.22 parts of the 1: 1 chromium complex of the dye of the formula 0.82 parts of the 1: 1 chromium complex of the dye of the formula and 1.05 parts of the 1: 1 chromium complex of the dye of the formula and 1.28 parts Na2SiF6 in 1000 parts of water, the dye liquor is kept at 50 ° for 10 minutes and then heated to 98 ° at a rate of 1 ° / minute. The pH at the beginning of dyeing is 4.
• the dye liquor After adding a solution of 2.15 parts of the 1: 1 chromium complex of the dye of the formula 0.98 parts of the 1: 1 chromium complex of the dye of the formula 0.45 parts of the 1: 1 chromium complex of the dye of the formula and 0.46 parts of the 1: 1 chromium complex of the dye of the formula the dye liquor is kept at 50 ° for a further 10 minutes and then heated to 98 ° at a heating rate of 0.8 ° / minute. The pH at the beginning of dyeing is 3.8. After 90 minutes of dyeing at 98 °, the mixture is cooled to 50 ° and the dye liquor is drained off. The brown-colored wool yarn is rinsed at 50 ° for 10 minutes, then at room temperature and dried as usual. The medium brown color obtained is excellent in fiber and has good fastness properties.
• Example 7 800 parts of worsted wool are in a dyebath containing 20 parts of water at 50 °, 64 parts of sodium sulfate, 1.1 parts of Na2SiF6, 32 parts of acetic acid (80%) and 12 parts of the leveling agent used in Example 6, while Pretreated for 15 minutes at 50 °.
• the dye liquor After adding a solution of 1.88 parts of the 1: 1 chromium complex of the dye of the formula 1.74 parts of the 1: 1 chromium complex of the dye of the formula 0.82 parts of the 1: 1 chromium complex of the dye of the formula and 1.05 parts of the 1: 1 chromium complex of the dye of the formula the dye liquor is kept at 50 ° for 10 minutes and then heated to 70 ° at a rate of 1 ° / minute, held at 70 ° for a further 20 minutes and then heated to 85 ° at 1 ° / minute.
• the pH at the beginning of dyeing is 4. After 120 minutes of dyeing at 85 °, the mixture is cooled to 50 ° and the dye liquor is drained off.
• the brown-colored wool yarn is rinsed at 50 ° for 10 minutes, then at room temperature and dried as usual.
• the full brown color obtained is excellently fibrous and has good fastness properties.
• a yarn dyeing with the same dyes according to the above procedure, but without the addition of Na2SiF6, is strongly fiber-uneven and significantly weaker.
• the dye liquor After adding a solution of 2.7 parts of the 1: 1 chromium complex of the dye of the formula 0.43 parts of the 1: 1 chromium complex of the dye of the formula 0.45 parts of the 1: 1 chromium complex of the dye of the formula and 1.8 parts of the 1: 1 chromium complex of the dye of the formula the dye liquor is kept at 50 ° for a further 10 minutes and then heated to 70 ° at a rate of 1 ° / minute, held at 70 ° for a further 20 minutes and then heated to 98 ° at 1 ° / minute.
• the pH value at the start of dyeing is 3.7.
• After 90 minutes of dyeing at 98 ° the mixture is cooled to 60 ° and the dye liquor is drained off.
• the navy blue dyed wool yarn is rinsed twice for 10 minutes at 50 °, then for 5 minutes at room temperature and dried as usual.
• the marine dyeing obtained is excellently fibrous and has good fastness properties.
• EXAMPLE 9 100 parts of woolen fabric are placed in a dyebath which contains 8 parts of sodium sulfate, 1.5 parts of the leveling aid given in Example 1 and 2.6 parts of 85% formic acid in 1500 parts of water at 40 ° for 10 minutes at 40 ° pretreated. The pH is 3.7. After adding a solution of 0.17 parts (NH4) 2SiF6 and 0.09 parts of the 1: 1 chromium complex of the dye of the formula 0.076 parts of the 1: 1 chromium complex of the dye of the formula and 0.4 parts of the 1: 1 chromium complex of the dye of the formula the dye liquor is kept at 40 ° for a further 10 minutes and then heated to 70 ° at a heating rate of 0.8 ° / minute.
• the dye liquor After 10 minutes of dyeing at 70 °, the dye liquor is heated to 100 °. After 90 minutes at 100 °, the mixture is cooled to 60 ° and the dye liquor is drained off. The gray-colored wool fabric is rinsed for 5 minutes at 50 °, then at room temperature and dried as usual.
• the dyeing obtained has excellent fiber shelf properties and good fastness properties.

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• 1987
  • 1987-09-30 US US07/102,942 patent/US4818248A/en not_active Expired - Lifetime
  • 1987-10-05 EP EP87810571A patent/EP0264346B1/de not_active Expired - Lifetime
  • 1987-10-05 ES ES198787810571T patent/ES2030094T3/es not_active Expired - Lifetime
  • 1987-10-05 EP EP91104413A patent/EP0443631A1/de not_active Withdrawn
  • 1987-10-05 DE DE8787810571T patent/DE3777746D1/de not_active Expired - Lifetime
  • 1987-10-08 NZ NZ222093A patent/NZ222093A/xx unknown
  • 1987-10-08 CA CA000548856A patent/CA1302017C/en not_active Expired - Lifetime
  • 1987-10-09 JP JP62253952A patent/JPS63105193A/ja active Granted
  • 1987-10-09 ZA ZA877607A patent/ZA877607B/xx unknown
  • 1987-10-09 AU AU79523/87A patent/AU608778B2/en not_active Ceased
  • 1987-10-10 KR KR1019870011227A patent/KR960003085B1/ko not_active Expired - Fee Related
• 1994
  • 1994-10-20 HK HK114794A patent/HK114794A/xx not_active IP Right Cessation

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