DE131567C - - Google Patents

Description

IMPERIAL

PATENT OFFICE.

In the patent 113893 a method for the representation of cotton direct black-coloring sulfur dyes, which consists in the fact that the through Effect of chlorosulphur on aniline, its salts, phenol or cresol of the trade obtained body on aromatic polyamido or oxyamido derivatives (especially p-phenylenediamine, p-amidophenol and o-p-diamido-p'-oxydiphenylamine) react. ·

The inventor has now found that when this process is used on certain of the substances listed in that patent, by changing the working conditions, namely maintaining temperatures of 140 to 150 ⁰ , blue or violet-blue, cotton directly blue and violet-blue dyeing can be obtained.

Example I. One reduced 150 parts of the indophenol obtained by oxidation of an equimolar mixture of p-phenylenediamine and phenol with 500 parts of cold water in dissolved sodium sulphide, then slowly heated to about 120 to 130 ^0th When this temperature is reached, 225 parts of the reaction product of chlorosulphur and phenol are added. One then heats the mixture of the two substances for two hours at 130 ⁰ and then läfst the temperature to rise gradually, without departing from 140 to 150 ^0, but in such a way, that evaporating the water and a dry mass is that the new dye forms and can be consumed directly in this form. This dye is very soluble in water with a blue color; it is completely precipitated from its solution by acids, but the precipitate is soluble in caustic soda and, above all, in alkaline sulfur. The latter solutions or the aqueous solutions of the raw product dye unheated cotton a beautiful blue.

In this example, the product of chlorosulfur and phenol can be replaced by the product Substitute from chlorosulfur and commercial cresol.

Example II. Instead of the indophenol used in Example I, one can also use that from Use indophenol obtained from p-phenylenediamine and o-cresol.

160 parts of this indophenol are reduced with 300 parts of sodium sulphide dissolved in cold water. The mixture is heated slowly to 120 to 130 ⁰ and sets, as soon as the mass became pasty, 200 parts of the Prod'uctes of chlorine and phenol to sulfur. Then the mixture is heated for three hours at 140 to 150 ⁰ until completely dry.

The dye is obtained in the form of a black color that is sparingly soluble in water, but in powder that is easily soluble in water mixed with caustic soda or sodium sulphide.

The dissolved dye can be used to dye cotton directly.

In this example, the product of chlorosulfur and phenol can be replaced by the replace from chlorosulfur and cresol. c

The table below shows the main properties of the new process obtained dyes compiled.

Main properties of the new dyes.

the one with Schwefelna
trium preserved
ductionsproduct of the
Indophenols from:
p-phenylenediamine and
phenol
p-phenylenediamine and
o-cresol - Appearance Solution in water with: Caustic soda the
previous
solutions
give with
an acid
treated The precipitate obtained by the acid
is with: sulfur
sodium
jo pCt. sulfur
acid
66 ° B. nitrous
more substantial
sulfur
acid Discoloration I2.pCt. Product made from chlorosulfur and
Phenol with: the one with Schwefelna
trium preserved
ductionsproduct of the
Indophenols from:
p-phenylenediamine and
phenol
p-phenylenediamine and
o-cresol black
black sulfur
sodium dark blue
dark
violet Precipitation
Brown
black
Brown
black Caustic soda
₄ o ° B. dark blue
Brown
violet sparingly soluble
deep blue
Brown
black dirty
violet
black ι pCt. blue
violet blue Product made from chlorosulfur and
Cresol with: black
black blue black
brown purple blackish
violet
dark
violet .Brown
black
Brown
black insoluble
insoluble black
violet
Brown
purple. deep purple
black dirty
red-violet
greenish
black blue-gray
violet gray blue
violet. black- ·
violet
purple brown insoluble
insoluble blue-gray
red-gray

Claims (1)

Patent claim:
Process for the preparation of blue and violet-blue sulfur dyes, characterized in that the products of action of chlorosulphur on phenol or commercial cresol on the indophenols reduced with sodium sulphide from p-phenylenediamine and phenol or cre, sol in the presence of sodium sulphide at temperatures of 140 takes effect up to 150 ^0.