SU55850A1 - Method for producing sulphurous blue dye - Google Patents

Description

The invention relates to the field of obtaining sulfur blue dyes.

It is known that when sulphite or bisulphite is exposed to indoiilins simultaneously with their reduction to the leuco-form, the sulfonation reaction proceeds.

This is how bisulfite reacts with indoaniline: p-hydroxy-p-dimethylamino-diphenylamine, p-phenylamino-p-oxydiphenylamine, dinitroxyphenylamine, etc.

The authors exposed indoaniline: p-aminotolyl-roxyphenylamine to bisulphite, and a product was obtained which in its properties was different from leuco-indoaniline (p-amidotolyl-p-oxyphenylamine).

When sulphite is treated with a condensation mass resulting from the action of nitrosophenol on o-toluidine in a sulfuric acid medium, a light gray product that is not oxidized in air is released.

The resulting product was subjected to a sulfonation of polysulfide in various temperature conditions from 105-120 ° to various amounts of polysulfide from 1.5 to 2.54 moles per 1 mole of organic matter and different composition of polysulfide: Na2S4 and NajSs.

In contrast to the sulfur dye obtained from p-amidotolyl-p-hydroxyphenylamine, the sulfurification of the product of bisulfite exposure produces a sulfurous blue dye, the colors of which correspond to the grades ZK or 2K of sulfur blue 2B (from p-ami1 dotolyl-p-oxyphenylamine).

The dyeing of the sulphurous blue 2B is considerably dumber, greener and harder than the brands ZK and only after the treatment with sodium hydroxide and the dye release by blowing air twice with air, corresponding to one of the brands ZK. or 2K. The product of the sulfonation of the bisulfite compound is not released from the water by blowing air and lisses are released on salting out. Thus, the sulphurization of the product of the bisulfite effect on the aforementioned indophenol makes it possible to produce a sulfurous blue dye in the form of a melt.

Example 1. Preparation of a bisulfite product with p-amidotolyl-p-hydroxyphenylamine.

539 g of sulfuric acid (5.5 moles), 89 g of water, 107 g of p-toluidine are loaded into a leaded pot equipped with a leaded broom.

(, mol) And at a temperature of + 5 ° to -f 10 °, 123 g of nitrosophenol (1 mol) are powdered over 4-5 hours.

The resulting condensation mass is poured onto a solution of sulfite, prepared in leaded apparatus from 1088 g of NaaSO. 7 H2O (4.12 mol) in 4000 g of water and ice to maintain the temperature not higher than 5 °.

Light gray product precipitated from the acidic medium is filtered off.

Example 2. Aging of the product of the reaction of bisulfite with p-amidotolyl-p-hydroxyphenylamine.

198, 12 g lOOVo-ro are loaded into an iron cooking pot supplied with a stirrer, thermometer sleeve and cooler. NazS (2.54 mol) as an 18Vft solution of 324 g of sulfur (10.12 mol) and after 2 hours

stirring at a temperature of 90-95 load on the prepared polysulfide paste product obtained in example I.

The melt is evaporated to a temperature of 120 °; when this temperature is reached, the refrigerator is reversed, and at the same time, acronenia is maintained for 10-15 hours.

Dyeing with water corresponds to one of the grades of sulfur blue 2B.

The subject matter of the invention.

The method of producing blue sulphurous dye by heating 4-aminotolyl-4-oxyphenylamine with polysulfide, characterized in that prior to the sulphurisation, 4-aminotolyl-4-oxyphenylamine is treated with a sulphite solution at a temperature not higher than + 5.