SU327221A1 - METHOD OF OBTAINING CUBE DYES - Google Patents

Description

This invention relates to the field of making new vat dyes suitable for dyeing a purple cube of cotton fiber in various ways in colors ranging from yellow-orange to red.

A known method for the production of vat dyes derived from the namylene tetracarboxylic acid diamide by reacting the perylenetetracarboxylic acid dianhydride with the amino derivatives of the aliphatic and aromatic series in the quinoline medium in the presence of concentrated hydrochloric acid, followed by isolation of the target product by known techniques.

The resulting dyes from a red-violet hydrosulfite cube stain cotton fabric from yellow-orange to red and in other colors.

In order to obtain vat dyes with more interesting shades, higher color indices, as well as their possible use as organic pigments for varnishes, plastics and for dyeing chemical fibers in the mass, a method of obtaining new vat dyes, consisting of that peril-1,, s, y-thiophene-3,4,9,10-tetracarboxylic acid is reacted with primary amines or ammonia in an aqueous medium in the presence of surfactants, followed by release Target product known prpemami. The use of a new raw material, in particular, peril-1,2-, c, / -thiophene-3,4,9,10-tetracarboxylic acid, allows not only to obtain dyes with good color characteristics that are different from those based on perylenetetracarboxylic acid But, it allows to expand the range of raw materials, i.e., it allows to improve the range of vat dyes.

Example 1. Suspension 4.22 g (0.01 mol) peril -1.12 - b, c, d - thiophene-3,4,9,10-tetracarboxylic acid (thieno-PTC), 3.69 g

(0.03 mol) p-apizidine and 12 g of sodium chloride in 120 ml of water are heated for 8 hours at 100 ° C and vigorous stirring; a sample is taken, diluted with water, then boiled with a 10% caustic potassium solution. The absence of blue fluorescence in the sample treated with an alkaline solution indicates that the reaction is complete. The reaction product is cooled to 50 ° C and filtered. The resulting bright orange paste is boiled with 150 ml of 1% hydrochloric acid for 1 hour, filtered at 50 ° C, washed with water until neutral according to Congo. The paste is then boiled with 100 ml of a 10% potassium hydroxide solution for 30 minutes, cooled.

until neutral and dried at 90 ° C, 5.9 g (93.5%) of the D 2 dye will be obtained.

A sample for analysis is prepared by boiling a dye with nitrobenzene and subsequent filtration, washing with a syrt and drying.

Found,%: 54.81; N4.20.

Calculated,%: S 4.96; N 3.87.

In concentrated sulfuric acid, the solution becomes purple. Dye from a violet cube colors cotton fabric in orange color.

Example 2. A solution of 1.05 g (0.0022 lolo) of thieno-ntc and 0.8 g of a dispergator of NF in 80% of a 5% solution of methylamine is boiled with stirring and a 20% aqueous solution of methylammonium is added periodically ( only about 20 ML) within 20 hours. The reaction is completed if the sample taken at boiling with a 10% KOH solution does not give a bright blue fluorescence.

The red suspension obtained is filtered, washed with water, treated with 1% potassium hydroxide solution, as described above. This gives 1.087 g (yield 94.0%) of dye No. 1, which is a yush, it is a dark red powder that does not dissolve in water and organic solvents.

In concentrated sulfuric acid, the solution becomes purple. Dye from a violet cube colors cotton fabric in red color.

Example 3. A suspension of 1.05 g (0.0022 mole) of tcno-Pdc 0.9 g (0.01 mol / n-toluidipa, 0.3 g of dispersant NF and 4 g of sodium chloride in 40 ml of water is heated for 21 hours at boiling. The reaction is carried out as described in example 1. 1.35 e (yield 90%) of dye No. 3 is obtained, which in its color indices resembles dye 2.

In a concentrated sulfuric acid solution, it acquires a purple color; from a purple cube, the dye paints cotton fabric in a yellow-orange color.

Example 4. A suspension of 1.05 g (0.0022 mol} thieno-PTC, 0.9 g (0.01 mol) / g-toluidine, and

0.3 g of NF dispersant in 30 ml of water is closed in glass amula and heated for 8 hours at 140-150 ° C. The reaction is completed if the sample is taken at boiling with a 10% KOH solution and does not give a bright blue fluorescence. The treatment of the suspension obtained is carried out as described in Example 1. 1.38 g (91.5%) of dye 3 are obtained.

The dye from the purple cube colors cotton fabric in yellow-orange color.

Example 5. A suspension of 1.05 g (0.0022 g) of thieno-PTC, 2.4 ml of 20% methylamine and 0.3 g

NF dispersant in 30 ml of water is closed in a glass ampoule, heated at 140 ° C for 9 hours. The determination of the end of the reaction and the isolation of the dye was carried out in the same way as described in Yrimer 4. Obtain 1.07 g (yield 92.1%) of Dye No. 1.

Example 6. A suspension of 1.05 g of thieno-PTC, 4.25 ml of a 20% aqueous solution of ammonia, 0.3 g of dispersant NP in 30 ml of water is sealed in a glass ampoule and heated at

140C for 9 hours. The reaction is carried out similarly to that described in Example 4. 1 g of dye is obtained (yield 90%). In concentrated sulfuric acid, the solution becomes purple. Violet dye

Cube dyes cotton fabric in red.

Subject invention

A method for producing vat dyes, characterized in that. In order to obtain dyes with high color indices, as well as their possible use as organic pigments for varnishes and plastics, peril-1, s, a1-thiophene-3,4,9,10-tetracarboxylic acid is reacted with primary amines or ammonia in a water medium in the presence of surfactants with the subsequent release of the target product by known methods.