DE137078C - - Google Patents

Description

IMPERIAL

PATENT OFFICE.

M 137078 CLASS 22 b.

In Section III of Patent 86539 ^ it is reported that when purpurin sulfonic acid is condensed with aromatic amines with elimination of the sulfo group, water-insoluble dyes (purpurin mono- and dialphylides of Patent 86150) are formed.

It has now been found that under certain conditions it is possible to initiate the reaction so that the sulfo group is retained, resulting in water-soluble sulfonic acids which can be used directly as dyes. Here is the course the condensation also surprising insofar as apparently the alphylido groups in other Enter position, which emerges from the various properties of the bodies represented in this way.

Namely while z. B. the sulfonic acids of the above-mentioned Alphylidoanthraquinones Patent specification 86150 dyeing unheated wool red to gray-violet creates the new products a clear, intense blue on unheated wool.

In order to represent the new products, the reaction conditions are to be chosen in such a way that before the start of the condensation, the separation of the condensation causing the condensation in a different sense Sulpho group does not occur, which is apparently associated with the formation of the well-known alphylidoanthraquinones from purpurinsulfonic acid by the method of patent 86539 of Case is.

This aim is best achieved by the condensation taking place at lower temperatures, e.g. B. at 90 to 120 ⁰ , is carried out.

One proceeds z. B. as follows:

Example.

10 kg of purpurin sulfonic acid are used in 100 kg added molten p-toluidine, added 10 kg of boric acid and the whole thing while stirring heated to 90 to 120 °. The initially yellow-red color of the melt goes here first in red violet, then in blue violet. When the purpurin sulfonic acid disappeared the melt is poured into dilute hydrochloric acid, the precipitate is filtered off and washed acid free and dries. The condensation product is thus obtained in the form of a dark blue powder, which is obtained by recrystallizing, z. B. from aniline, obtained purely as dark blue needles or prisms, which are in aniline, Dissolve pyridine and so on with blue color, in sulfuric acid with yellow color and the p-toluidine salt of the new dye sulfonic acid. By heating said p-toluidine salt with

125666.

Previous additional patents: 86539, 89090, 91149, 91150, 95625, 101805, 101806, 114199, 116867,

dilute soda solution, the salt goes into solution, whereby p-toluidine is expelled. From the above solution, after acidification with dilute acetic acid, the sodium salt of Dye can be obtained by salting out. When moist it is dark blue Paste, dried, is an indigo blue, shiny copper powder that dries in cold water difficult to dissolve in hot water. With the addition of caustic soda, this solution becomes violet, with an excess of pure blue. The solution in concentrated sulfuric acid is yellow and is not significantly changed with boric acid. This reaction distinguishes the new product is characteristic of the Purpurinmono- or. -di-ptoluidid the patent specification 86150, which bezw in sulfuric acid with red-violet. green-blue color, which when boric acid is added in blue green respectively. Transition to blue-violet.

The dye stains wool in an acid bath in clear blue tones, which are obtained by after-chroming turn into a real green. Alumina-stained wool becomes pure blue, chrome-stained Wool dyed green-blue. The dyeings are very lightfast.

Completely analogous compounds are obtained if the condensation is used instead of p-toluidine other aromatic amines are used.

Instead of boric acid, the others in patent specification 86150 find mentioned condensation agent use.

The following table summarizes the properties of some representatives of this body class.

Condensation product
the end: cone.
sulfur
acid Solve 1
sulfur
acid and
Boric acid λ η gsmi
alcohol 11 e 1 '
Pyridine aniline A.
on un
more heated
Wool coloring
on for-
chromir-
ter wool η
acid
coloring
after-
chromized Purpurin sulfonic acid
+ Aniline red-yellow red-yellow red
violet violet violet violet reddish
Gray blue-gray Purpurin sulfonic acid
+ p-toluidine yellow yellow blue blue blue blue green Blue green Purpurin sulfonic acid
4 ~ m -xylidine yellow yellow violet
blue blue violet
blue blue
violet green Blue reddish
Gray Purpurin sulfonic acid
+ p-phenetidine yellow yellow blue greenish
blue greenish
blue blue green Blue green.

Claims (1)

Patent claim: The by claim 2 of the patent, one DAF in order to avoid cleavage of the sulfo group, the condensation at lower temperatures, zweckmäfsig not more than 120 ⁰ 86539 performs modification-protected method for the condensation of aromatic amines with Purpurinsulfosäure, consisting.