CH95509A - Process for the preparation of a new sulfur-containing dye. - Google Patents

Description

  

  Process for the preparation of a new sulfur-containing dye. The invention is based on the observation that new sulfur-containing dyes, probably thiazines, are formed when ss-ogynaphtoquinonarylimino compounds of the general formula:
EMI0001.0004
    are treated with sulfur, and its object is a process for the preparation of such a sulfur-containing dye by treating ss-ogynaphthoquinone-p-chloroanilide
EMI0001.0008
    with sulfur.

   This treatment of the P-oxynaphthoquinone-p-chloroanilide can advantageously take place in such a way that it is carried out directly with sulfur, with or without the addition of a carrier, in the presence or absence of a solution, or respectively. Diluent is heated, or is exposed to the action of sulfur dissolved in SCLE or in fuming sulfuric acid at temperatures that are not too high, or is brought together with sulfur dissolved in alkaline sulfur at low temperatures, advantageously in an alcoholic solution.



  <I> Example 1: </I> 10 kg of p-oxynaphthoquinone-p-chloroanilide
EMI0001.0016
    are intimately mixed with 20 kg of sulfur, 50 kg of naphthalene and 0.2 kg of iodine sulfur or iodine and heated to the boil for several hours. To remove the naphthalene, the melt xpit of hot naphtha is extracted and the remaining residue is freed from sulfur in a known manner, for example by digestion with sodium sulphide solutions.

   The product obtained in this way is expediently converted into a paste that can easily be vetted by dissolving it in concentrated sulfuric acid and pouring this solution onto ice, and as such is used directly for dyeing and printing. When dried, the dye is a dark violet powder, with a dark violet color soluble in concentrated sulfuric acid. From the yellow-colored hydrosulphite vat, wool is dyed violet-black, and very real blue-green colorations are created when chromium plating.

    <I> Example 2: </I> 8 kg of sulfur flowers are gradually introduced into 200 kg of oleum with 300/9 SOa content at 20-300 C. As soon as the sulfur has dissolved, 10 kg of p-oxynaphtocbinone-p-chloroanilide are gradually added with thorough stirring, stirring is continued for several hours at 30-400 ° C. until the reaction is complete, then poured onto ice, filtered and washed the filter material is neutral. The paste obtained in this way is, if necessary, freed from excess sulfur and used immediately in this form. The dyestuff shows very similar physical, chemical and coloring properties to that obtained according to Example 1.



  <I> Example 3 </I> 10 kg of ss-oxynaphthoquinone anilide are introduced into a mixture of 60 kg of glacial acetic acid and a solution of 10 kg of sulfur in 23 kg of SCP with stirring; the mixture is stirred for a few hours at ordinary temperature. then warms up and allows the reaction to end at an elevated temperature. The precipitated dye is filtered off and converted into a readily soluble paste that can be used immediately for dyeing by dissolving it in concentrated sulfuric acid and pouring it onto ice. The dye shows the same properties as that obtained in the previous examples.

 

Claims (1)

PATENT CLAIM: Process for the production of a new sulfur-containing mordant dye, characterized in that, Q-Oxynaphthoquinone-p-chloroanilide EMI0002.0024 treated with sulfur. The dye forms a dark purple powder that dissolves in concentrated sulfuric acid with a dark purple color. He dyes wool from the yellow-dyed hydrosulfite vat violet-black; very true blue-green colorations are obtained on post-bromination. SUBCLAIMS: 1. Process according to claim, characterized in that the treatment with sulfur consists in direct heating with sulfur. 2. The method according to patent claim and un teran claim 1, characterized in that the reaction takes place in the presence of a diluent. 3. The method according to patent claim and un teran claim 1, characterized in that the reaction takes place in the presence of a solvent. 4. The method according to patent claim and un teran claim 1, characterized in that the reaction takes place in the presence of a sulfur carrier. 5. Process according to patent claim, characterized in that the treatment with sulfur consists in that the β-oxynaphthoquinone-p-chloroanilide is exposed to the action of a solution of sulfur in SCl 'at a temperature that is not too high. 6. The method according to claim, characterized in that the treatment with sulfur consists in that the ss-oxynaphthoquinone-p-chloroanilide is exposed to the action of a solution of sulfur in fuming sulfuric acid. 7th Process according to patent claim, characterized in that the treatment with sulfur takes place by combining the ß-ogynaphthoquinone-p-chloroanilide with sulfur dissolved in alkaline sulfur at low temperatures. 8. The method according to claim and un teran claim 1, characterized in that the reaction takes place in alcoholic solution.