DE1070762B - PROCESS FOR THE PREPARATION OF GRAY SULFUR DYES OF THE PHTALOCYANINE SERIES - Google Patents

Description

Subject of patent application C 14807 iVb / 22d is a process for the production of gray sulfur dyes of the phthalocyanine series, which is characterized by is that on phthalocyanines or their complex salts hydroxylamine or hydroxylamine supplying substances, and chlorosulfonic acid in the presence of compounds of the elements of V. and VT. Group of the periodic table at elevated temperatures below 100 ° C lets act and the reaction mixture in the same temperature range with at least 5 moles of chlorosulfur, based on phthalocyanine.

In a further development of this inventive concept it has now been found that dyes of more ncutral gray instead of olive gray nuance with even better lightfastness if you get about 50 to 90 ° / o of the quantity of chlorosulphonic acid used there replaced by sulfuric acid monohydrate.

example 1

in a mixture of 276 parts by weight of sulfuric acid monohydrate and 69 parts by weight of chlorosulfonic acid are successively 23 parts by weight of copper phthalocyanine, 0.3 parts by weight of ammonium molybdate and stirred in 15.6 parts by weight of hydroxylamine sulfate and heated to 80 to 85 ° C for about 20 hours, the originally yellow-olive solution color after Moss green turns. 40.5 parts by weight of chlorosulphur are then left in for 10 to 15 minutes run in and stir for 2 to 3 hours at the same temperature. After cooling to about 30 ° C the reaction mixture is stirred into 5 to 6 times the amount of ice water. A gray-black precipitate is obtained, which is filtered off with suction and washed neutral and is dried. The dye obtained in this way dissolves in concentrated sulfuric acid light green, in aqueous sodium sulphide solution with a blue-green color and dyes cotton from it in gray tones of good washability and excellent lightfastness.

Example 2

11.5 parts by weight of copper phthalocvanine and 0.11 parts by weight Ammonium molybdate is added to a mixture of 173 parts of chlorosulfonic acid and 17.3 parts Sulfuric acid monohydrate entered. After adding 9.8 parts by weight of nitromethane is within 6 to 6V2 hours heated with stirring to 85 ° C and then 20 hours at the same Method of manufacture

of gray sulfur dyes

the phthalocyanine series

Addition to additional patent application C 14807 IVb / 22 d
(Auslegeschrift 1 067 154)

Applicant:
Cassella Farbwerke Mainkur

Corporation,
Frankfurt / M.-Fechenheim

Dr. Heinrich Ritter and Dr. Eberhard Stier,

Frankfurt / M.-Fechenheim,
have been named as inventors

Temperature stirred. The further treatment with chlorosulfur and work-up takes place according to the example 1. The dye obtained in this way dyes the textile fiber from a dirty black-gray sulfur sodium solution in slightly yellowish olive-gray tones than the dye obtainable according to Example 1.

P A T E N T Λ N S P H I j C 11:

Further development of the process for the production of gray sheep dyes Phthalocyanine series according to patent application C 14807 IVb / 22d, characterized in that here on phthalocyanines or their complex salts hydroxylamine or hydroxylamine-supplying substances in a mixture of about 50 to 90 parts by weight of sulfuric acid monohydrate and about 50 to 10 parts by weight of chlorosulfonic acid in the presence of compounds of the elements V. and Vl. Group of the Periodic Table at elevated, but below 100 ° C temperatures can act and that reaction mixture in the same temperature range with at least 5 mol of sulfur chloride, based on phthalocyanine, further treated.

A coloring table was displayed when the application was announced.

909 688/369 12.59

Claims (1)

FEDERAL REPUBLIC OF GERMANY CO 9ß GERMAN kl INTERNAT. KL. C 09 b / 08, _ ' PATENT OFFICE EDITORIAL 1 070 ' C 16689 IVb / 22 d / V NO REPORTING DAY: APRIL 19, 19SB NOTICE
THE NOTICE
AND ISSUE OF THE
EDITORIAL: DECEMBER 10, 1959