DE274489C - - Google Patents

Description

IMPERIAL

PATENT OFFICE,

PATENT LETTERING

- M 274489 CLASS 22 β. GROUP.

From the patent specification 114634 it has become known that a number of dis- and polyazo dyes with resorcinol in the end position can be made washable by treating their dyeings with formaldehyde. The one in this However, the dyes cited in the patent give only dark brown to black nuances; lively tones are completely absent.

It has now been found that such vivid red to blue dyes are obtained when 2 molecules of an acidyldiamine or a nitroamine are diazotized with 1 molecule of a product obtained by the condensation of two molecules 2 · 5 · 7-aminonaphthol sulfonic acid arises, such as the urea of 2 · 5 · 7-aminonaphthol sulfonic acid or 5 · 5'-dioxy-2 · 2'-dinaphthylamine-7 · 7'-disulfonic acid couples, the resulting dyes are saponified or reduced, further diazotized and finally with 2 molecules Resorcinol, m-diamines or m-aminophenol or their derivatives are coupled. The with help of 5'5'-dioxy-2 · 2'-dinaphthylamine-7-7'-disulfonic acid produced dyes have the valuable property when developing with diazotized p-nitroaniline on the fiber very washfast and easily etchable black dyeings to deliver.

Example 1.

27.2 parts of m-aminoformanilide are diazotized with the aid of 60 parts of concentrated hydrochloric acid and 13.8 parts of nitrite. This diazo solution is then allowed to run into a solution of 54.8 parts of the urea of 2.5 · 7-aminonaphthol sulfonic acid (sodium salt) in 2000 parts of water and 40 parts of calcined soda. The mixture is stirred for 12 hours, then heated to 90 ° and 150 parts of sulfuric acid of 40 ⁰ Be are used. to, one receives another ¹ J ₂ hours at this temperature, allowed to cool to 60 ° and sucks off the dye.

The sucked off dye is mixed with 2000 parts of water, weakly with sodium hydroxide solution made alkaline, cooled to 10 °, then with 60 parts of hydrochloric acid and 13.8 parts of nitrite offset. The mixture is stirred for 6 hours. Then allowed to run into a cooled to 0 ° Solution of 22 parts of resorcinol in 1000 parts of water and 60 parts of calcined soda. Man heated to 60 to 70 ° and salted out the dye with table salt. He dyes cotton yellowish red.

In this example, the m-aminoformanilide can be replaced by other acidyl-m-diamine, z. B. 4-formyl-2 · 4-tolylenediamine, 2-formyl-2 · Replace 4 - toluenediamine, 4 - formyl -2-4- diaminoanisole, etc., without anything substantial to change the procedure.

Likewise, instead of resorcinol, m-phenylenediamine or m-aminophenol, etc. use.

Example 2.

30 parts of p-aminoacetanilide are in the usual manner with 60 parts of hydrochloric acid 1.16 specific gravity and 13.8 parts sodium nitrite diazotized. The diazo solution is allowed to run into a solution cooled to 0 °

Solution of 5,6,5 parts of 5-5'-dioxy-2-2'-dinaphtylamine-7 · ¹ J ¹ I- disulfosaurem sodium in 100 parts. Water and 42 parts of calcined soda. After -.- I to 2 hours is boiled, treated with 300 parts of sodium hydroxide solution of 33 percent, and still cooks I ¹ Z ₂ to 2 hours. Then, neutralize with hydrochloric acid and salt out the 'dye. The dye is squeezed out. 'The press cake is stirred with 1500 parts of water, made weakly alkaline with sodium hydroxide solution, cooled to 10 ° and diazotized with 60 parts of hydrochloric acid and 12 parts of nitrite. Stir until the nitrite disappears. A solution of 16 parts of hydrochloric acid m-phenylenediamine is then added and the mixture is made clearly alkaline with soda, heated to 60 to 70 ° and the dye is salted out. It dyes cotton a reddish blue.

Example 3.

52 parts of oxalyl-p-phenylenediaminesulfonic acid are diazotized with the aid of 60 parts of concentrated hydrochloric acid (specific weight 1.16) and 13.8 parts of sodium nitrite and the diazo compound is converted into an ice-cold solution of 50 parts of 5 · 5'-dioxy-2 · 2 ' -dinaphtylamine-7 .7'-disulfonic acid (sodium salt) given in 1000 parts of water and 42 parts of soda. The mixture is stirred for 1 to 2 hours and, after the addition of 300 parts of a 33 percent sodium hydroxide solution, a further ¹ /. _i hour heated to 90 °. Then it is neutralized with hydrochloric acid, salted out and filtered off. The dye obtained is then stirred with 1500 parts of water with the addition of a little sodium hydroxide solution, cooled to 10 ° and further diazotized with 60 parts of hydrochloric acid and 13.8 parts of nitrite Parts of soda are added, the mixture is heated to 60 to 70 ° and the dye is salted out and filtered off. It dyes cotton blue, after treatment with diazotized nitraniline on the fiber black.

Instead of m-phenylenediamine, resorcinol, m-aminophenol, take m-toluylenediamine, etc., instead of p-aminoacetanilide, other acidyldiamines, such as 2-oxalylamino-5-amino-p-xylene, 2-amino-5-acetylaminotoluene, 2 - oxalylamino-4-chloro-5-amino-i-anisole, 2-oxalylamino-4-methyl-5-aminoanisole, acidyl -1 · 4 -naphthylenediamine · 6-sulfonic acid, etc. without changing anything substantial in the process.

Claims (1)

Patent claim: Process for the representation of nouns Polyazo dyes ^ consisting in that the diazo compounds of 2 molecules of an acidyl diamine or 2 molecules of a nitroamine with 1 molecule of the urea of 2x5x7-aminonaphthol sulfonic acid or 1 molecule of 5 · 5'-dioxy-2 · 2'-dinaphthylamine-7 · 7'-disulfonic acid is coupled, the dyes saponified or reduced, further diazotized and with 2 molecules of resorcinol, m-diamines or m-aminophenol or their derivatives.