SU192214A1 - METHOD FOR OBTAINING ACTIVE STYRILTRIAZINE DYES - Google Patents

Description

This invention relates to the field of active dye production.

Enocq6 is proposed for the preparation of active styryl triazine azo dyes of the general formula

SN CH-SbND

N

s-sx

. J-NH /

sOsH DI

BUT 7J

.gl

/ -.

SOgH

where NH is in position 1 or 6; X -No or COOH;

YI and Ya - H, C1, CH;), not previously described in the literature. Dyes of this type on the cellulose fiber are yellow and lemon yellow in color, which have good resistance to the action of a soap solution at 100 ° C and sweat, which ensure the formation of a chemical bond dye fiber.

The dyes are obtained by the condensation of 2-styryl-4, 6-dichloro-1, 3, 5-triazine with a. Myazole of the general formula

C-CX

SOsH

where NHj is in position 1 or 6;

X, YI and Ya are as defined above,

with phenylenediaminosulfonic acid followed by a combination of the condensation product with

pyrazolones.

Example 1. 1.38 g of 2-steryl-4,6-dichloropl, 3,5tripasine, dissolved in 15 ml of acetone, is mixed with e 2.48 g of a mn of uranium dye, dissolved in 90 ml of water and obtained from diazotiropena acetylmetafenylene diaminesulfonic acid and 1-phenyl-3-1methyl-5-pyrazolone-51 sulfonic acid, followed by distillation of the acetyl group. The reaction is carried out at 40 ° G,

and pli is not higher than 7, preferably at pH 4.5-5, tide as necessary 1 pp soda solution. The process is considered complete when the pH change ceases or the diazotizing fluid with the amgp-group disappears. The dye is precipitated by the addition of 10 g of salted salt and filtered.

The dye paste is mixed with 0.6 g of mono-potassium phosphate and 0.3 g of disodium phosphate n is dried in vacuum at 70-75 ° C. The yield is 6.5 g with a content of red, its substance is 47.5% (counting on a mol. Century 712.5), which is 87% of the theoretical value, based on an aminomonazo dye.

The resulting dye stains cotton fabric in yellow with a clean shade; the degree of fixation when dyeing from a long bath is good.

Example 2. 1.38 g of 2-styryl-4,6-dichloro-1,3,5-triazine, dissolved in 20 ml of acetone, is added to 1.13 g of metaphenylene diamine sulphonic acid, dissolved in 90 ml of water. The reaction is carried out at 30 ° C and RP no higher than 8, preferably with a pH of 4.5-5, tide as needed 1 n. a solution of sheloche. The process is terminated when the pH change ceases. The solution of the acylated product is filtered from non-admixture impurities of excess dichloride or dioxo compound, cooled to O - minus 2 ° C, and 4.5 ml of 4 N are added to it. hydrochloric acid solution and diazotize, pouring 3 ml 2 n. solution of sodium nitrite but as the latter disappears. In the process of diazotization, 3 g of salt is added to coagulate the diazo compound. Suspension of the diazo compound is added at the same temperature for 30 minutes to 1.9 g of 1- (2-chloro-5-sulfophenyl) -3-methyl-5-pyrazolone dissolved in 20 ml of water 13 ml of 2N. soda solution. The mixture is stirred for 2 hours, the dye is precipitated with 5 g of salt and filtered.

The dye paste is kneaded with 0.4 g of mono-potassium phosphate and 0.2 g of disodium phosphate and dried in vacuum at 70 ° C. Yield 2.82 g, which is 75% of theory, considered metaphenylene diaminesulfonic acid; co-concentration of 50%.

The resulting dye paints cotton fabric in pure yellow with a greenish tinge; the degree of fixation and strength to sweat and soap solution at 100 ° C is good.

Example 1.51 g of 2-styryl-4,6-dichloro-1,3,5-triazine, dissolved in 20 ml of acetone, is mixed with 6.11 g of 46.4% (0.05 g-mol) amino-compound, dissolved in 90 ml of water and obtained from diazotized acetylmetaphenylene diamine sulfonic acid and 1- (2, 5-dichlorophenyl) -3-methyl-5-pyrazolone-4-sulfonic acid, followed by acetyl cleavage. The reaction is carried out at 40 ° C and pH 5-6, tide as necessary 1 n. soda solution. After the change in RP has ceased, the dye is precipitated by addition of sodium chloride and filtered.

The dye paste is kneaded with 0.6 g of mono-potassium phosphate and 0.3 g of disodium phosphate and in vacuum at 70 ° C. The yield is 4.98 g with the content of the coloring substance determined by the method of reduction with divalent vanadium salts, 52%. The yield from the theory is 70%, taking into account amino amino compounds. The content of total chlorine is 22.2%, chlorine-ion is 14.9%, covalently bound chlorine is 7.3% ,. The content of covalent bound chlorine was calculated for C27Hi9O7N8S2Cl3, i.e. 14.43% for 100% dye and -7.51% for 52%.

The resulting dye is well fixed by cotton fiber when dyeing from a long bath and gives yellow tinges with a greenish tint.

Example 4. The reaction is carried out, similarly to that indicated in Example 1, using an aminoazo compound obtained from diazotized acetylmetafenylene diamine sulphoxy acid and 1-phenyl-3-carboxy-5-pyrazolone-4-sulphonic acid, followed by cleavage of the acetyl group.

The dye dyes cotton fiber yellow with a less greenish tint than in example 3.

Example 5. The reaction is carried out, similarly to that indicated in Example 1, using aminoazo-compound obtained from diazotized acetyl-para-phenylenediamine-sulfonic acid and 1-phenyl-3-methI and T-5-pyrazolone-5-sulfonic acid, followed by cleavage of the acetyl group.

Dye paints cotton fiber yellow with a reddish tinge.

Under conditions similar to those described above, other stryltriazine dyes from meta- or para-phenylenediamine sulphonic acids and other, not mentioned above, derivatives of pyrazolone are produced.

Example 6. When applied in a crash, the dye is rubbed into a paste with a large amount of cold water, diluted with warm water (40-50 ° C) at a ratio of water to weight of the fabric to be dyed to 30: 1.

The cellulose fibers are dyed in a neutral dye solution for 15 minutes at 40-45 ° C, then sodium chloride (20-70 g / l) is added in two doses and dyed for 30 minutes at 40-45 ° C, after which t sodium phosphate (10-20g / l) and continue dyeing for 60 minutes at 40-45 ° C. Finally, they are washed, washed for 5 minutes at boiling in a solution of deer soap (5 g / l), washed with hot and cold water, and dried.

Example 7. When printing is applied, the dye, taken in an amount of 10-50 g per 1 kg of printing ink and mixed with urea (30-100 g / kg), is dissolved in hot water with a temperature of 90 ° C (450-335 ml ), add a sodium algnate thickener (500 g), cool the printing ink to room temperature and add sodium bicarbonate (10-15 hours). The fabric is printed with the prepared printing ink, dried, steamed in a brew at 102-105 ° C for 2-3 minutes, washed in cold water, washed for 5 minutes by boiling in a solution of olein soap (5 g / l), washed with hot and cold water and dry.

Subject invention

The method of obtaining active styryl triazine dyes of the general formula

CH CH-SeN5

N: NC-CX

 with N RG N

eo n

where NH is in position 1 or 6; YI and Y, -H, C1, CH3;

X - CH3 or COOH, characterized in that, in order to expand the range of active styryltriazine dyes, 2-styryl4, 6-dichloro-1, 3, 5-triazine is condensed with an aminoazo dye of the general formula.

N Nc-s's

SOjH with, N BUT Vf

th

SO, H

20

where NHo is in position 1 or 6; Yub Y2 and X are as defined above, or with phenylenediaminosulfonic acid, followed by a combination of the condensation product with pyrazolones.