SU4166A1 - A method of producing sulfuric acid esters of leuco compounds and using them for dyeing and stuffing fibrous materials, as well as producing lacquers from them - Google Patents

Description

Instead of conventional leuco compounds, the bottoms dyes are proposed to be used in dyeing and printing, as well as water-soluble salts of the sulfate enol esters of leuco compounds for the manufacture of varnishes.

For the preparation of sulphate esters of leuco compounds, the dry leuco compounds are treated with chlorosulfonic acid in the presence of any tertiary base. Example 1. K 72 wt. including cooled pyridine, gradually added 17.6 wt. including chlorosulfonic acid and then 12.5 weight. including dry di-hydro-indigo. The mixture is kept in an atmosphere of neutral (carbon dioxide) gas and stirred first in the cold and then at 50-60 ° C for / g-1 hour. At the end of the reaction, -10 volumes of water are diluted, lightly sown, and filtered. A crystalline salt appears, which is to be added to another more

1b.

Example 2. 100 g of dry leuco compound from 5: 7: 5: 7 tetrabromoindigo are introduced into a cooled to 0 ° mixture of 44 g of chlorosulfonic acid, 100 g of dimethylaniline and 300 g of chlorobenzene. After stirring for two hours at ordinary temperature, the mixture is gradually heated to 60 ° and after half an hour it is made w ith, fir-tree with help, and caustic soda, and the mixture of dimethylaniline and chlorobenzene in it is distilled off with water vapor. From the remaining and filtered solution by the addition of sodium chloride, sulphate is salted out as it quickly solidifies its oil.

Example 3. 156 g of dry leukothoindigo are introduced into a cooled to 0 ° mixture of 134.5 g of chlorosulfonic acid, 280 g of dimethylaniline and 500 g of chlorobenzene. The mixture is constantly stirred. When it reaches room temperature, it is gently heated to 60 ° for two hours, making it tartaric with gumosh and caustic

soda and dimethylaniline and chlorobenzene are distilled off with water vapor. From the resulting filtered and evaporated solution, the ether crystallizes out.

EXAMPLE 4 100 g of benzoyl-1-amino-anthraquinone are reduced with 120 g of hydrosulfite and 240 g of 30% sodium hydroxide, and the leukosulphate is precipitated with acid as a yellow precipitate. The latter is filtered off, dried and in a dry form introduced into a mixture formed by adding dropwise 200 g of chlorosulfonic acid to 1000 g of dimethylaniline (or another tertiary base) at a low temperature. At the end of the reaction, the amount of soda needed to form the sodium salt is added and distilled with water vapor. From the remaining clear transparent solution, the sodium sulfate is salted out in the form of yellow crystals with sodium salt.

Example 5. 100 g of di-chloro-dianilido-benzoquinone, obtained by the action of analyte on chloroaniline (see Lieb, Japp. 114, p. 306), is reduced with 100 g of hydrosulfite and 200 g of 30% sodium hydroxide, precipitated by the addition of acid the corresponding substituted hydroquinone in the form of white crystals. The latter are sucked off, present and added to a mixture of 220 g of chlorosulfonic acid and a tertiary base, for example, 1000 g of dimethylaniline. At the end of the reaction, a quantity of soda (400 g), necessary for the formation of a salt, is added and subjected to distillation with water vapor. The remaining liquid is filtered, sodium chloride is added, after which the sodium salt crystals of dichloro-dianilido-hydroquinone sulphate ester are precipitated in the form of thin oblong plates.

Example 6. 100 g of indanthrene (M-dihydro-1-2-1-2 - dianthraquinonazine) is reconstituted in the usual way and the corresponding leuko-compound is precipitated with acid. The leucosilane, which is saturated in the absence of air, is introduced into a mixture of 350 g of chlorosulfonic acid and 2000 g of dimethylaniline at 0-4 °. The mixture is stirred for several hours at ordinary temperature, after which a sufficient amount of soda is added to neutralize it and distilled with water vapor. Little is produced during the reaction. soluble red product whose solubility increases with the addition of soda.

The compounds obtained are soluble in water, either by themselves or as a solution, constant. Their aqueous solution does not change from the addition of alkalis; mineral acids decompose them slowly in the cold and faster at elevated temperatures. Weak oxidizing agents in the presence of acids translate them into the original dye; in air, this transformation occurs due to the action of light rays. Compounds are best consumed. in the form of neutral bodies, such as, for example, metallic salts, and not in the form of free acids, less constant than salts.

Dyeing and printing of the obtained sulfate esters of leuco compounds and obtaining lacquers from them are as follows.

Solutions of the salts of these esters are applied to a paper or woolly fabric or are mixed with the substrate, and then carried out on a weak acid with the addition of some oxidizing agent FeClg, CdSgOO, NaNOg, etc., or without it. The ester is washed and oxidized to a dye that adheres firmly and quickly to the fiber.

An example of the manufacture of varnish. A solution containing 12 kg of Glauber's salt in 120 liters of water precipitates in the cold with a solution of 20 kg of cold barium in 200 liters of water. This precipitate is agitated, containing 6.2 kg g of leucoindigo ester. After that, sulfuric acid