DE59868C - Process for the preparation of stain-coloring dyes from alkylated amidobenzophenones - Google Patents

Description

IMPERIAL

PATENT OFFICE.

By condensation of alkylated amidobenzophenones with dioxynaphthalene or pyrogallol by means of phosphorus oxychloride a number of valuable stain-coloring dyes are obtained, with which one can achieve new, since then unattainable coloring effects. Condensations of phenols (phenol, resorcinol, α- and ß-naphtol) with tetraalkyldiamidobenzophenone are already, following the steps disclosed in Patent No. 27789 laid down invention, in patent no. 31321 of August 21, 1884 has been described. However, the products presented according to the latter are completely useless, and also the subsequent treatment of these with ammonia, amines, etc. for the preparation of purely basic triphenylmethane dyes, which form the actual aim of the last-named patent has never led to its technical exploitation.

In contrast to this, the condensation products represented by the new process are usable immediately; these belong to the class of stain-coloring dyes, by z. B. on chrome-stained wool or cotton in magnificent purple to color blue-green shades.

The most valuable results have since been obtained from the condensation of tetramethyl and Tetraethyldiamidobenzophenone with 1) dioxynaphthalene (2x3), 2) dioxynaphthalene (1x2), 3) dioxynaphthalene (2 x 7) or 4) pyrogallol. Phosphorus oxychloride has proven to be a condensation agent best proven.

The procedure is essentially the same for all of the above compounds is explained by the following example:

100 kg of tetramethyldiamidobenzophenone will be heated with 200 kg of phosphorus oxychloride on a water bath for 10 minutes. Then 60 kg of dioxynaphthalene (2 x 3) of patent no. 57525 registered and the mass was kept at water bath temperature for 2 hours with thorough stirring. The cooled melt is then cautious dissolved in 250 1 3% acetic acid, the solution poured into water, the deposited Dye is filtered off and washed out with water.

In this way the dye is obtained as a black-blue paste, which can be used directly for the Printing and coloring can be used. When dry it presents a red-brown, Crystalline, metal-shining powder, which is difficult to convert in cold water into easily dissolves in hot water. The solutions in alkali carbonate and free alkali are blue, those colored green in concentrated sulfuric acid. On chrome-stained wool or cotton it gives beautiful blue nuances.

The dye from dioxynaphthalene (2 x 7) forms a blue-black, metallic-luster powder; the same thing The solutions in alkali carbonate are difficult to dissolve in cold water and easily soluble in hot water and free alkali are stable and have a pure blue color. In concentrated The body dissolves sulfuric acid with it

yellow color. On chrome-stained wool or cotton, it delivers lively green tones.

The dye from dioxynaphthalene (1-2) shows same appearance as that from dioxynaphthalene (2-3); he differs from this by its insolubility in alkali carbonate and free alkali and by the violet-blue color of its solution in concentrated sulfuric acid. The staining on chrome-stained Wool or cotton are gray-blue.

To prepare the dye from pyrogallol, an excess must be used in the condensation of pyrogallol apply. The dye forms a blue-black powder; in cold Water is heavy, and only soluble in traces in hot water. The color of the sulfuric acid The solution is red-yellow, the solution in alkali carbonate is violet, in free alkali it is dirty-red and inconsistent. The dye dyes chrome-stained wool or cotton purple.

The dyeings of all these dyes on unheated wool are far weaker and more cloudy than those produced on wool prepared with the usual stains will. ■ ■

The bezw in an analogous manner from Tetraäthyldiamidobenzophenon and the Dioxynaphtalinen. Pyrogallol dyes show the same properties as the analogous ones from Tetramethyldiamidobenzophenonen obtained.

The dye from dioxynaphthalene (2 ■ 3) is a reddish-brown, crystalline, metallic luster Powder, difficult in cold water, easily soluble in hot water. The solutions in alkali and Alkali carbonates are colored blue, those in concentrated sulfuric acid are colored green. On chrome-stained It delivers beautiful shades of blue for wool or cotton.

The dye made from dioxynaphthalene (2 · 7) forms a blue-black, metal-shining powder; the same thing is difficult to dissolve in cold water, easily soluble in hot water; the solutions in alkali and Alkali carbonates are permanent and blue in color. Dissolves in concentrated sulfuric acid the body with yellow color.

On chrome-stained wool or cotton, it delivers lively green tones. ■

The dye from dioxynaphthalene (1 x 2) forms a red-brown, shiny copper, crystalline powder; in alkali carbonate and free It is insoluble in alkali, just as it is in cold water, while it dissolves somewhat in hot water. In concentrated sulfuric acid it dissolves with a violet-blue color.

The colors on chrome-stained wool or cotton are gray-blue.

The dye from pyrogallol is difficult to dissolve in cold water and more easily soluble in hot water. He represents a blue-black powder, which in concentrated sulfuric acid is mixed with yellow-red Color dissolves. The solution in alkali carbonate is violet, that in free alkali violet-red and inconsistent. The dye dyes chrome-stained wool or cotton purple.

Claims (4)

Patent claim: Process for the preparation of violet to blue and green stain-coloring dyes by condensation of tetramethyldiamidobenzophenone or tetraethyldiamidobenzophenone and one of the following phenols, namely: 1. dioxynaphthalene (2 x 3), 2. dioxynaphthalene (1 '■ 2), 3. dioxynaphthalene (2 x 7); 4. Pyrogallol by means of phosphorus oxychloride.