DE87935C - - Google Patents

Description

IMPERIAL

PATENT OFFICE.

By the action of an aromatic amine such as aniline on the hydrochloric acid salt of Gallocyanin dye, which is produced by the reaction of hydrochloric acid diethylamidoazobenzene or Hydrochloric acid nitrosodiethylaniline on gallamic acid is obtained - at an exposure temperature from 40 ° to 60 ° C. - a new dye, which differs from the already known Condensation products of aniline with gallocyanin dyes, such as gallocyanin, Prune, gallamine blue, etc., distinguishes itself by the fact that it has green-blue nuances on chrome stains supplies, while the latter color in reddish-blue shades and an advantageous commercial one Allow use only by converting them into sulfonic acids.

This difference is due, on the one hand, to the fact that the new dye is represented the hydrochloric acid salt of the gallocyanine dye used and on the other hand the reaction at is carried out at a lower temperature, while for the representation of the condensation products described earlier of aniline with gallocyanine dyes (cf. Ber. XXI, p. 1745, and XXV, P. 2995, as well as the patents No. 55942 and No. 57453 etc.) the gallocyanine dye as ■ Base used and the condensation was carried out at a higher temperature.

Example:

10 kg of the hydrochloric acid salt of the dye obtained by the action of hydrochloric acid or hydrochloric acid Diäthylamidoazobenzol Nitrosodiäthylanilin on Gallaminsäure are heated with 20 kg of aniline for approximately one hour and with constant stirring at 50 ⁰ C.. After standing for a day and cooling the mass, it is filtered, the dye obtained in this way and only slightly soluble in alcohol is washed out with alcohol to remove the last traces of aniline, pressed and dried, or the mass is poured into hydrochloric acid water after the reaction is complete neutralize the excess aniline with hydrochloric acid, filter, press and dry.

For its commercial use, the dye can be converted into sulfonic acid. It is, however, more advantageous to use it without prior conversion into sulphonic acids, since it colors in shades that are more lightfast and waterfast than its sulphonic acids. For this purpose, the purified Condensationsproduct is dissolved in twice its weight amount usually sulfuric acid at a temperature below 50 ⁰ C. and general the dye solution thus obtained with stirring, mälig into cold, event, poured a salt-containing water, wherein the dye as a fine precipitate precipitates, which is obtained in dough form after filing and is used directly in the printing and dyeing works. He dyes chromed wool in an acid bath in green-blue lightfast and milled shades.

. In order to obtain a yield that approximates the theoretical yield in the preparation of the new dye care must be taken to ensure that

1. the dye as condensate with aniline hydrochloric acid taken and

2. The condensation is carried out at a temperature of ⁰ to 40 ° C. 6o.

From the following table are some of the main characteristics by which the obtained Condensation product from the original dye, as well as from others Condensation prod icts of the latter Aniline is different, obviously.

Dye off
Gallamic acid
+ hydrochloric acid
ethylamidoazobe
zol or hydrochloric acid
Nitroso diethyl
aniline Hydrochloric acid salt
of the dye,
condenses with
Aniline at 40 ⁰
up to 6o ° C. Base of the color
fabric, condens
sirt with aniline
at 40 ° to 60 ° C. Hydrochloric acid salt
of the dye,
condenses with
Aniline at 150 ⁰
up to i6o ° C. Base of the color
fabric, condens
sirt with aniline
at J5O ° to
i6o ° C. Solubility in con-
centered sulfur
acid Blue solution that
by adding
Water in red
transforms Rothe solution,
which by access
set of water
in yellow over
goes Bluish reddish
Solution that
by addition
of water in
red passes Red violet
Solution that
by addition
of water in
reddish yellow
transforms Violet blue
Solution that
by addition
of water in
violet-tinged
red passes Solubility in salt
acid Rothe solution Yellowish
solution Rothe solution Rothe solution,
by
Addition of
Water in yellow
transforms Red-brown
Solution that
by addition
from water to
yellowish over
goes Solubility in
water Red violet
solution Insoluble Insoluble as
Base. By
Addition of
Acid rothvio
lette solution Insoluble Insoluble Added vinegar
acid to watery
solution The coloring of the
Solution goes in
red over Remains insoluble Red violet
solution Remains insoluble Little blue
colored solution Added vinegar
acid to an al
alcoholic solution The coloring of the
Solution turns red The coloring
the solution
goes from blue
into yellowish
above The coloring
the solution
turns red Remains largest-
partly insoluble.
Little blue ge
colored solution The coloring
the solution
goes in blue
above.

To that of the dye base and aniline at 40 ⁰ to 6o ° C: shown Condensationsproduct is to be noted, that it is a great measure is made of non-wandelter dye base and chromirte wool in röthlichblauen nuances stains, while at 150 ⁰ to I6O ° C. illustrated Condensationsproduct from the Dye base and aniline represent a mixture of several bodies and dye chromed wool in dirty reddish-blue shades. On the other hand, the condensation of the hydrochloric acid salt provides the dye with aniline at a temperature of 150 ⁰ to 160 ⁰ C. a very low yield of dye and is the Condensationsproduct obtained, chromirte wool in dirty grünstichigblauen nuances stains, a great measure of a resinous mass.

Claims (1)

Patent Claims: Process for the preparation of a blue-green, stain-coloring dye by heating aniline with the hydrochloride of the or by the action of hydrochloric acid nitrosodiethylaniline. hydrochloric acid diethylamidoazobenzene. Gallocyaninfarerstoff.es obtained on gallamic acid at a temperature of 40 ⁰ to 60 ° C. Conversion of the condensation product obtained by the process of claim 1 into a paste that can be used directly for dyeing and printing by dissolving the same in ordinary sulfuric acid at low temperature and pouring the solution thus obtained in cold water.