DEP0002859DA - Process for the production of sulfur dyes - Google Patents

Description

JMDANNER
Dr.W.ZERWECK

Dr "Bu / St. Frankfurt a / M-Fechenheim, September 10th 1948

Process "for the production of sulfur ar '

It has been found that valuable Sulfur Dyes can be obtained by using bodies of the phenanthrazine series in themselves in a known manner with sulphurizing agents, if necessary with the addition of copper compounds, and the raw material thus obtained melt opens up in the usual way. :.

The dyes obtained in this way color the vegetable fibers from the sodium sulphide bath in valuable shades of good color Authenticity properties, especially a remarkable Lieht® © authenticity. ·

Example,!, I ₁ ; :

In a solution of 12 parts of sulfur in 170 parts of chlorine sulfur are at 60 ° 20 parts of phenanthrazine of the formula

gradually entered. The temperature is then increased to about 150 ° and the mixture is kept on the reflux condenser for about 2 hours Tea temperature held. The chlorosulfur is then distilled off, the residue is dried and baked for several hours at 270-280 °. After the raw product has been broken down in the usual way, a dye is obtained which is derived from the vegetable fiber from the sodium sulphide colors the bathroom bright yellow-brown with very good fastness properties,

Example 2s

20 parts of toluphenanthrazine (6-methyl-1.2.S «, 4 - = - dibeszophenaziR) are gradually added to a melt of 12 parts of sulfur in 100 parts of chlorosulfur and 3.2 parts of benzidine added. It is heated slowly to about 150 °, refluxed for 1 hour and distilled then dries to dryness. Then the temperature is raised to about 270 ° and held at this level for about 8 hours. Through post-treatment * The dye is broken down with sodium sulfate and then

worked up. It colors the vegetable fiber from the sulphurous sodium bath yellow-brown.

If the melt is carried out in the presence of Ktipfersulfid _s , a darker yellow-brown coloring material is obtained.

Example 3; ,,

Substituting in Example 1, the Phenasthrazin by Chiaoxal "phtaanthrazin (Beilstein, 4th edition, Vol _{9 e} 26, Ste _39G)? in this way, a dye is obtained which dyes the vegetable fibers from the sulfur-sodium bath a pungent brown.

Example 4 .; >. _P.

S-Nitrophenanthra ^ phenazine (Beilstein ^. Auf 1, _f Volume 23, St @ 330 treated according to Example 1, results in a dye that dyes the vegetable fibers from the sodium sulphide bath dark brown.

Example 5;

Judging from 6-nitro-l. £ .3 "4-dibenzophenazin and v @ r ^ drives the rest of Example I ₉ is obtained a dye cotton from the Sehwefelnatriumbade stained brown.

Example 6;

10 parts Trinitrophenanthrazin _obtained} dureh Kitrierea of Phenanthrazin be entered at the boil in a Polysulfidsehmelze of 70 parts and 40 parts of crystallized Sehwefelnatrium. Is it refluxed for several hours at a temperature of 118 °? then the melt is dried, then the temperature is increased to 270 ° and held for about 8 hours at 270-280 °. After digestion of the crude product in the usual way, a dye is obtained which bathes the vegetable fibers from the sodium sulfate dark brown in color.

Claims (1)

Claim ι Process for the production of sulfur dyes, characterized in that one contains bodies of the phenanthrazine series in per se * known way with sulphurizing agents, if necessary with addition. of copper compounds, treated and the raw clay obtained in the process unlocks in the usual way "