SU600159A1 - Method of preparing active monochlortriazine copper-containing azo dye - Google Patents

Description

As a vyalivayuschey agent, use of a bovine salt in the amount of 1 -15% of the solution volume at pH 2.0-3.5 or the pigment of the target product in the amount of 1-2% of the volume of the reaction mass at pH 1.5-3.5.

Example 1

Diazotization of 2-aminophenol-4-sulfonic acids.

In a 250 ml flask equipped with a stirrer, a thermometer, 70 ml of water are poured, while stirring, 3.78 g of 2-aminophenol-4-sulfonic acid and 1.84 g of hydrochloric acid are charged and the mixture is cooled to 5-7 ° C. 1.46 g of sodium nitrite is charged to the temperature and kept for 1 hour. Then, excess nitric acid is removed with a 10% solution of sulfamic acid.

Combination with Ash-acid.

A 250 ml five-necked flask equipped with a stirrer, thermometer, glass and calomel electrodes is charged with 40 ml of water, 7.18 g of Ach-acid and cooled to 0 -2 ° C, the pH is adjusted to 8.0 at this temperature. ammonia water and add diazocompound, maintaining a constant pH of 8.0-8.2 and a temperature not higher than 8 ° C. Then the mixture is kept for 2 hours. With a positive analysis at the end of the combination, copper plating is carried out.

Copper plating of azo dye.

In a flask with a capacity of 250 ml, equipped with a stirrer, a thermometer, load azo dye solution and copper ammonia, previously prepared from 20 ml of water, 4.3 g of copper sulfate and 2.71 g of ammonia water at 30-40 ° C. Copper plating is carried out for 1.5 hours at 18-20 ° C, after soaking with hydrochloric acid, the pH is adjusted to 3.0-3.5, salt is loaded in an amount of 15% of the solution volume, stirred for 1 hour and filtered. Azo dye paste is acylated with cyanuric chloride.

Acylation

In a 250 ml five-necked flask equipped with a thermometer, an-mixer, glass and calomel electrodes, 130 ml of water are charged, the copper azo dye paste is dissolved at pH 6.0. Into the cooled mixture up to 2-4 ° C, 0.23 g of the preparation of OS 20, 3.5 g of cyanure chloride is charged and the pH is adjusted to 6.5. Allow 1 hour and determine the end of the acylation (chromatographic).

Amination and isolation of the dye.

In a flask with a capacity of 250 ml, where the acylation took place, 1.63 g of ammonia water was charged, heated to 40 ° C and held for 2 hours. Then the pH was adjusted to 2.5-3.5, heated to 60 ° C. and filtered. The finished dye paste is stabilized with 10% disodium phosphate and dried. The weight of the dry dye is 17 g, the yield is 80%, the dye concentration is 160-190%, 1000 / o-dye is 11.3 g. The resulting dye is dyed cotton fiber in purple color. In terms of quality indicators, the target product corresponds to MRTU No. 6-14-238-69.

Example 2. The procedure was carried out under the conditions of Example 1, but after the azo-coagulation of the azo-dyes, the reaction mixture was directly acylated, excluding the stages of isolation, filtration, and azo-redissolution. The output of the dye, counting on 2-aminophenol-4-sulfonic acid, 95%. In terms of hue, purity corresponds to the type sample, the dye concentration is 130-150%.

Example 3. The experiment was carried out under the conditions of Example 1, but the finished dye was isolated with 2% pigment at a pH of 2.5-3.5. The output of the dye 80%. In hue, purity, the dye corresponds to MRTU No. 6-14-238-69. The ink concentration is 160% relative to the type sample.

Example 4. The experiment was carried out under the conditions of Example 2, but the isolation of the finished dye was carried out at a pH of 1.0-1.5 without the addition of salt, followed by stabilization and drying. The yield of the dye is 81.0%, calculated on 2-aminophenol-4 sulfonic acid. In color and purity, the dye corresponds to the type sample.

The proposed method allows to increase the yield of the target product to 80-95% versus 49.2% of the known, i.e., 30-45%; reduce the duration of the technological process at the stage of isolation to 1 hour versus 20-30 hours as known; due to the complete elimination of the use of table salt or the reduction of its consumption by half (for example, at the present time, salting out 1 ton of the finished product consumes 4.5 tons of high-quality “Extra” brand salt) to drastically reduce the salinity of industrial waste and thus repeated use in the process.

In terms of shade and purity, the target product corresponds to MRTU No. 6-14-238-69, and exceeds the typical sample by 60-90% in coloring concentration.

The economic effect from the introduction of the target method will be about 61,000 rubles per year in terms of raw materials.

Claims (1)

Invention Formula The method of obtaining active monochlorotriazine copper-containing azo dye by combining pre-diazotized with a further 3-aminophydephenol-4-sulfonic acid with Al-acid followed by treatment of the azo compound thus obtained with copper ammonium, by acylation of the copper complex of the azo compound with cyanur chloride, followed by aminazation with triaze 3 characterized in that, in order to increase the yield and color concentration of the target product, the techno-intensification logical process and reduce the salinity of wastewater, the selection of the target product is carried out at a pH of 1.0-3.5. 5 Sources of information taken into account in the examination of the Technological regulation No. 280 for the production of dye active violet 4K D 334, p. 2, N ° 9689. Archive Merged “Dye.