SU883109A1 - Method of producing active metal-containing monoazodye - Google Patents

Description

The invention relates to the technology of producing azo dyes, in particular, to methods for producing active monochloro-triaainic metal containing monoazo dye used to dye cotton fabrics, natural and synthetic fibers. A known method for producing an active metal-containing dye by diazotizing 4-nitro-2-aminophenol, followed by combination with Al-acid at pH 8.0-8.5 in water, metallization with chromium salts, acylation, amination, isolation of the desired product in a neutral environment 1. The disadvantage of this method is the low yield of the target product (6 70%) and low - color concentration, as well as the duration of the process (48 hours). The closest technical solution to the present invention is a method of obtaining active metal-containing monoazo-dye by diazotization of 4-nitro-2-aminophenop, followed by combining with Ai-acid without prior dissolving it at pH - & O, by chromium salts metallization, acylation, separation Target Pro The product yield is 83%, the process duration is 48 hours. The disadvantage of this method is the low yield of the target product, low. as well as a large amount of wastewater. The purpose of the invention is to increase the yield of the target product, its color concentration, reducing the amount of wastewater. This goal is achieved by the fact that according to the method of obtaining the active me-. tall-containing monoazoxyphenol is synthesized by 4-nitro-2-amyiophenop followed by a combination with Al-acid, metallization, acylyropane, amination, precipitation of the complete product, and the metallization is subjected directly to the reaction mixture and the separation of the yellow product is processed. after the amination with a mixture of sodium chloride and capi, taken in an amount of 5-20 wt.% at pH 4-5 and. To completely eliminate wastewater, the reaction mass obtained after the amination stage is neutralized to a pH of 5-6, stabilized and dried. Example 1. By diazotization of 4- -nitro-2 aminophenol, its dissolution and purification. . A flask with a capacity of 100 ml, equipped with a stirrer and a thermometer, is charged with G, 89 g of 4-nitro-2-aminophenol, 17 ml of water, 0.88 g of hydrochloric acid and warming salt up to 40-50 C. At the same time, load 0, 13 g of activated carbon and stirred for 30 minutes, then filtered. A solution of 4-nitro-2-minophenol is obtained with a basic substance content of 100 g / l. 1.85 g of 1OO% product are obtained. Diazotization. In a 250 ml flask equipped with a thermometer, a stirrer, glass and calomel electrodes, the solution of 4-nitro-2-aminophenol obtained in the previous step is cooled to. When this temperature is reached, 0.83 g of sodium nitrite is charged and the temperature is maintained for 30 minutes. Upon completion of exposure, excess nitrous acid is removed with sulfamic acid. Combination with Ash-acid. To the resulting diazo compound was added 4.3 g of Al-acid 1 with 20 ml of water and the pH was adjusted to 8.0 by addition of 20% sodium hydroxide solution. After ZO, the minute mixing at a temperature not higher than 10 ° C and a thorough analysis at the end of the combination is carried out by metallization, after the neutralization of the reaction mass to pH 6.0 with hydrochloric acid. Chrome plating. The flask, where the combination took place and the monoazo dye was found, was heated to 90 ° C, after which chromium acetate was added, prepared by dissolving 0.86 g of chromium acetate in 7 ml of water. Heat the reaction mass to 10 -105.degree. C., maintain it for 2-3 hours at this temperature and pH 4-4.5, which is maintained with a solution of soda ash. 9 Cobalt. A solution of cobalt chloride prepared by dissolving 0, Q5 g of cobalt chloride in 7 ml of water is loaded into the reaction mass obtained at the chromium-plating stage and cooled to 80 ° C. The pH is adjusted to 10-10.5 with sodium hydroxide solution , stir 1 hour. At the end of the reaction with positive analysis at the end of the metal, the reaction mass is cooled to 10-15 ° C and neutralized to pH 6.0 with hydrochloric acid. Acylation In a solution of the metal complex, cooled to / 10 ° C, 5 ml of 25% ammonia water is loaded, heated to 0.1 g of the preparation OC-2O, 2.5 g of cyanuric chloride and the pH is maintained at 6, O-6.2. . At the end of the reaction, your lyration leads to amination. Amination To the reaction mass, where the acylation took place, 5 ml of 25% ammonia water was added, heated to and kept at this temperature and pH not lower than 9.0 2 hours. After the end of the reaction, the reaction mass was acidified to pH 4 With hydrochloric acid and charged with a 20% mixture of potassium chloride and sodium chloride in a ratio of 1: 2, stirred for 1 hour, let the mixture stand for 2 hours and filter. The weight of the paste is 18 g. The dry residue is 9 g. The color is 150%. Yield 90%. The table shows examples of the preparation of the dye depending on the temperature, pH of the medium and the amount of salting-out. general agent. The proposed dye preparation method allows to increase the yield of the target product up to 9O-100% versus 83% of the known, halve the technological process, reduce the amount of saline wastewater three times or eliminate them completely by drying the dye solution, thereby eliminating , increase the dye concentration by 1.5-1.8 times, increase the solubility of the dye in water by 1.5 times.

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Claims (2)

No. 7 8831 Claims of Invention A method for producing active metal-containing mono-aerasis by diazotization of 4-nitro-2-aminophenop with the subsequent combination with Al-acid, metallation, acylation, amination, by dividing the desired product, in one. due to the fact that, in order to increase the yield of the target product, its effluent concentration, good wastewater, metallization is directly applied to the reaction mass after. combining and separating the chain product is carried out by treating the reaction mass after amination with a mixture of sodium chloride and potassium chloride, taken in an amount of 5-20 wt.% at pH 4-5 and 5-15 ° C. Sources of information taken into account in examination 1, Patent of Poland No. 724744, cl. From O9 To 15/01, pubic. 1974 2. USSR author's certificate No. 730766, cl. From 09 To 62/08, 1930 (prototype).