The method of obtaining the acid yellow monoisocyanates

C09B29/10 - from coupling components containing hydroxy as the only directing group


(57) Abstract:

The inventive method of obtaining acid yellow azo dye is combined diazotized metamelomai acid azo-components - resorcinolformaldehyde resin at a mass ratio of from 0.88 to 0.98 : 1, respectively, at 8 - 12C, and pH of 5.5 to 5.9. The yield of dye is 90 - 93,4% . Dye receive non-dusting form. table 1.

The invention relates to the field of aniline-dye industry, in particular to a method for acid yellow monoisocyanates (Dye acid yellow KIS), which can be used for dyeing fur sheepskin.

A method of obtaining dye acid yellow lightfastness 2G through a combination of protestirovanny sulfanilic acid with 1-(2,5-dichloro)-phenyl-3-methyl-5-pyrazolone-4-acid, separation and filtration of the obtained monoisocyanates, suspension pasta intermediate, sieving and drying the suspension of intermediate. The yield of 68.2% . The colour concentration of 120% .

The disadvantages of the above method are:

the low yield of the target product;

the formation of a large number of colored vysokomineralizovannoj deep paint over the skin (less than 1/3).

A method of obtaining acid monoisocyanates by combining diazotized amine (derived o-aminophenol) resorcinolformaldehyde resin in an alkaline medium followed by metallization of the target product.

The resulting dyes have tanning properties and do not color the hair.

The disadvantage of this method is the complexity of the technological process (the need for metallization).

The closest technological essence and the achieved effect is a method of producing dye acid yellow methylophaga by combining protestirovanny metamelomai acid with diphenylamine.

Metanovel acid diasterous at pH 1.0 and a temperature of 6aboutWith, then load the non and alizarin oil. To remove excess nitrous acid load solution of sulfamic acid. To the obtained diazoketone download solution of sodium acetate to pH 4.0, and then load the emulsion of diphenylamine at a temperature of 10-14aboutC. for 8 h serves soda ash to maintain a pH of 3.8. At the end of combination raise the pH to 7.0

After neutralization of the reaction mass, allocate target about the General concentration of 100% .

The amount of insoluble residue of 2.5% .

The disadvantages of the above method are:

the low yield of the target product;

the formation of a large number painted saline effluent 4300 kg/t containing dye 0.76 per cent , sodium chloride 18,9% , organic impurities of 0.16% , inorganic impurities 2,43% ;

when dyeing of fur sheepskin is significant coverage of the pile;

the complexity of the technological process due to the presence of stages of neutralization, separation, filtration and drying;

dye receive in the form of a powder, which leads to environmental pollution by dust dye.

The aim of the present invention is to increase the yield of the target product, simplifying the technology and improving the environment.

This objective is achieved in that in the known method, comprising the combination protestirovanny metamelomai acid azo-components, according to the invention, as azo-components used resorcinolformaldehyde resin and the combination is carried out at a mass ratio of diazotized Manilova acid: resorcinolformaldehyde resin equal to from 0.88 to 0.98: 1, respectively, at a temperature of 8-12aboutC and pH 5.5-5,9.

The essence of the proposed technical solution is illustrated by examples of specific implementation method.

P R I m e R 1. In a three-neck flask equipped with stirrer, thermometer, electrodes for measuring pH and bath for heating load 20 ml of water. Heat water to a temperature of 32aboutAnd loads of 1.65 g of resorcinol. Stir until dissolved and add 0,047 g of sulfuric acid to a pH of 1.5 pH unit. The mass is stirred for 20 minutes Then carefully added 2.7 g of formalin, ensuring that the temperature did not exceed 70aboutC. Maintain the temperature of the speed of the tide formalin.

After the download has completed formalin mass was incubated for 2 h with constant stirring and the temperature not more than 70aboutC. Select the sample for the qualitative analysis to determine the absence of formaldehyde. After holding the reaction mass was added 2.4 g of sodium hydroxide solution at a temperature of 80aboutWith up to a pH of 9.1 pH unit. Then the mass is cooled to a temperature of 20aboutC. Obtain a transparent viscous solution of sodium salt resorcinolformaldehyde resin.

Diazotization of metanias cooling. Download 60 ml of water and 8.76 g metamelomai acid, stirred until a homogeneous suspension. Then cooled to a temperature of 8aboutWith and add 2,19 g of hydrochloric acid up to pH 0.5 pH unit. Gradually add to 3.45 g of a solution of sodium nitrite by weakening the reaction of nitrous acid.

After adding all calculated quantity of sodium nitrite mass is stirred 1 hour at a temperature of 9aboutC and pH of 0.95 pH and low excess nitrous acid.

Immediately before the combination, the excess nitrous acid is removed 0,03 ml of sulfamic acid.

The combination is carried out in a beaker equipped with a stirrer, thermometer and electrodes for measuring pH. To 45 ml of a solution of sodium salt resorcinolformaldehyde resin cooled to a temperature of 10aboutC for 30 min, poured 40 ml of diazocompounds.

In pure witoka diluted and odolanow samples was visible a slight excess resorcinolformaldehyde resin (yellow staining with a solution of parameterdatabase). Diazoketone in solution were absent. The mass is stirred for 1 h, pH 5.5 pH. The final volume of 105 ml of the Obtained dye with a concentration of 22% , a density of 1.07 g/cm3. The total yield of 83.4% .

The proposed solution is compared with the prototype, has the following advantages:

increases the yield of the target product 8.1-13.2% of the (prototype - 80.2 per cent , on the proposed method to 88.3-93,4% );

the obtained target product has a tanning properties, desacralised pile;

reduced consumption of dye during the dyeing 15-20 times;

simplified technology by eliminating the stage of neutralization, separation, filtration and drying;

there are no painted saline wastewater;

the product is obtained in a non-dusting form. (56) production Process regulations dye acid yellow lightfastness 2G, N 127, N 1853.

USSR author's certificate N 609310, class 09 In 29/12, 1984.

Production process regulations dye acid yellow methylophaga, N 2144, IFESTOS, 1989.

The METHOD of OBTAINING the ACID YELLOW azo dye by combining diazotized metamelomai acid azo-components, characterized in that, to increase the yield of the target product, simplifying the technology and improving the environment, as azo-components used resorcinolformaldehyde resin and the combination is carried out at a mass ratio Diaz is


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