CS239541B1 - Process for preparing a blue metal complex complex dye - Google Patents

Abstract

The purpose is a more advantageous method of preparing a blue metal complex dye by azo coupling reaction of l-diazo-2-naphthol-4-sulfonic acid with 2-naphthol and subsequent chromization of the reaction product, which is achieved by azo coupling being carried out in the presence of a divalent zinc cation in the form of an amino complex in an amount of 1.10”2 to 1.10”1 mole per 1 mole of diazotization component.

Description

The present invention relates to a process for preparing a blue metal-complex-constitution

consisting of the azocopulation reaction of 1-diazo-2-naphthol-4-sulfonic acid with 2-naphthol and subsequent chroma-forming of the azo compound.

239 541

The methods currently used in the preparation of the aforementioned metallocomplex azo dye are based on the interaction of the diazotizing component 1-diazo-2-naphthol-4-sulfonic acid with the coupling component 2-naphthol in a weak acid to strong alkaliocome reaction medium. The resulting azo-dye is formed by various protruding agents. Due to the fact that the oloctrophilicity of the diazotization component is strongly influenced by the intra-molecular interacias of adjacent functional groups (-M * and N and -OH), a quantitative course of the azo coupling of the reaction cannot be achieved under these conditions. Another disadvantage of the hitherto used methods for the preparation of the dye of the constituent I. Another disadvantage is the need to remove the unreacted reaction components or their decomposition products, which would otherwise cause the shade deviation from the desired metallocomplex azo dye in the final metalocomplex dye. the desired shade and the bittering of some of its multi-color properties ·

It has now been found that the above disadvantages of the preparation of the constituent metal-complex dye of constitution I are eliminated by the process of azocopulation of a diazotization component which is 1-diazo-2-naphthol-4-sulfonic acid with a coupling component which is 2-naphthol. The composition according to claim 1, characterized in that the azocopulation is carried out in the presence of a bivalent monoclonal ml of zinc in the form of an amocomplex in an amount of 1 · 10 to 1 · 10 mol per 1 mol of diazotization component.

The process for the preparation of the metal-complex dye of constitution 1 according to the invention is carried out by adding aqueous solutions of inorganic salts of a bivalent mono-zinc cation to the reaction mixture before starting the azo coupling of the reaction conducted in an ammonia medium. It is preferred to use said condensation catalyst in the form of a pre-prepared zinc amine component by conversion of the corresponding halide, sulfate or nitrate by addition of aqueous ammonia solution. It is particularly preferred that the azo coupling of the reaction is carried out in the presence of alkali metal or ammonium carbonates or bicarbonates.

239,541 at relatively high temperatures, typically 50-100 ° C, to achieve a quantitative reaction while maintaining an equimolar ratio of reacting components. This in turn results in the creation of favorable conditions for the subsequent amazement of the product and the coupling of the reaction directly in the reaction mixture without isolation of the resulting azo compound by treatment with a suitable chromating agent, which is an advantage of the process of the invention. A further advantage of the process according to the invention is that the azo coupling of the reaction is achieved in a selective manner and a high yield of subsequent chromation is achieved, which in turn means a significant improvement in the coloristic properties of the final metallized product.

Example 1

Dissolve in 400 parts of water at a temperature of about 20 ° C

125 parts of ammonium 1-diazo-2-naphtho-4-sulfonic acid o.

salts. The Zn amocomplex prepared by dissolving 3 parts of ZnCl ₂ in 10 parts of water is then added to the solution followed by 18 parts of concentrated ammonia solution. The mixture was introduced into the coupling reactor with stirring with 72 parts of 4-naphthol, 250 parts of water, 45 parts of sodium carbonate and 10 parts of NaQH. The reaction mixture is maintained at 00 and 60 ° C for 1 h. After this time, a chromating reagent prepared by mixing 150 parts of hot water with 37 parts of potassium dichromate and 60 parts of oxalic acid is performed. The azo dye is chromatographed at about 95 ° C for 1h to give a 2: 1 solution of a metal-complex dye that dyees wool and PAD textiles to blue shades, from which the dye is obtained by drying in a spray drier.

Claims (1)

OBJECT OF TRANSMISSION 239 541 now A process for the preparation of a metal / complex dye constituting the azocopulation of a diazotization component which is 1-diazo-2-naphthol-4-sulfonic acid with a coupling component which is 2-naphthol and chromating the reaction product of the azocopulation, characterized in that it is:. azocopulaoe in the presence of divalent zinc cation in the form of amocomplex in an amount of from 1 to 10 mole per mole of diazotization component