DE226879C - - Google Patents

Description

IMPERIAL

PATENT OFFICE.

PATENT LETTERING

- ΛΙ 226879 CLASS 22 b. GROUP

the anthracene series.

Patented in the German Empire on March 5, 1909.

It has been found that the mercaptans or disulfides of anthraquinone in the treatment converted into new dyes with alkali polysulphide at a higher temperature, which differ from the disulfides in that they are alkaline hydrosulfite not to be reduced to the mercaptans, but to supply vats in which they are located let fix on the fiber. By rinsing

ίο or subsequent oxidation is obtained gray-brown to black-brown colorations of excellent fastness.

The conversion into the new dyes takes place by melting with alkali polysulphides with or without the application of pressure.

The mercaptans can also be replaced by those anthraquinone derivatives which are in the Sulfur-alkaline melt primarily mercaptans. remote, such as B. rhodanides and xanthates, or halides and sulfonic acids.

The dyes obtained in this way are brown to black powders, which in water, Alkali and alkali sulfur are insoluble. This is how they differ from the water-soluble ones Noun dyes of the patent specification 95484, which in part consist of the same Starting materials can be obtained with the help of alkali polysulphide.

Example 1.

5 parts of anthraquinone-i-mercaptan sodium are mixed with a solution of 8 parts of sulfur and 40 parts of crystallized sodium sulphide in 20 parts of water in a stirrer provided autoclave heated for 20 hours at 160 to 170 °. After cooling down it sucks one off and washed off with hot water. The dye forms a black powder, which is in pyridine with olive brown, in concentrated sulfuric acid with coffee brown Color dissolves. Its solution in alkaline hydrosulfite is brown. The ones made with it The colors are gray-brown to black-brown. The same result can be achieved with application from ι - Rhodananthraquinone, 1-chloroanthraquinone or from anthraquinone-i-sulfosaurem Potash.

Example 2.

ι part of anthraquinone - 2 -mercaptan sodium is mixed with a solution of 10 parts of potassium polysulphide (Sulfur liver) in 5 parts of water while slowly increasing the temperature fused from 150 to 200 ° for about 10 hours. By leaching with hot Water, the dye is isolated from the melt as a black powder. It is in organic solvents, as well as in concentrated form Sulfuric acid sparingly soluble. The brown vat provides gray-brown dyeings on cotton.

Example 3.

ι part of anthraquinone -1 · 5 - disulfonic sodium is heated with a solution prepared from 2 parts of sulfur, 10 parts of 28 percent sodium sulfhydrate and 7 parts of sodium hydroxide solution (34 ⁰ Be.) for 24 hours in an autoclave at 160 to 170 °. The by suction and

Wash out isolated dye forms a black powder that works in organic solvents insoluble, in concentrated sulfuric acid with olive-brown, in alkaline hydrosulphite is soluble with red-brown color when heated. The dyeings on cotton are reddish black-brown.

If you replace the anthraquinone disulphonic acid soda with anthraquinone-2-sulphonic acid soda or with 2-chloroanthraquinone, the dye of Example 2 is obtained.

The analog from i-aminoanthraquinone-5-sulfosaurem Soda-made dye gives a greenish black vat and a greenish tinge black-brown colorations.

Very similar products are obtained when using other halogen compounds or sulfonic acids of anthraquinone.

Claims (1)

Patent claim: Process for the preparation of gray to brown-black vat dyes of the anthracene series, consisting in the fact that one. Anthraquinone mercaptans or disulfides, or through alkaline sulfur in anthraquinone mercaptans transferable anthraquinone derivatives with alkali polysulphides via the one required for the formation of mercaptans Heated up to the temperature until water-insoluble dyes are formed.