SU12604A1 - The method of obtaining alkyl derivatives of sulfur-containing vat dyes - Google Patents

Description

Prepared according to known EPOs, by the action of sulfur or sulfur chloride on anthracene and its derivatives, dyes (such as indanthrenone, hydro-volatile and hydro-brown) have the property of producing brown alkali hydrosulfite, blue-violet, blue and dx. According to the proposed method, the products of reduction in an alkaline cube can easily be transferred, when interacting with alkylating agents, into new, no longer oxidizable compounds; these latter are intensely colored. The color shades approximate the color of the solution in a cube, but are completely different from the color of the original product. So, for example, from a reddish-brown dye, a dark blue dye is obtained when treating with ethyl bromide in a cube, and from the resulting olive-green dye (indanthrenolivka) with the same reaction is a black product.

As alkylating agents, all compounds used for this purpose are used, such as: alkyl halides, alkyl sulfates, gal: o-fat derivatives; acids and their esters, benzyl halide, then alkylating-acting fatty aromatic ammonium compounds, such as. for example, trialkylnaphthyl or dialkylbenzylaryl-ammonium salt, etc. The new dyes are valuable starting materials for the preparation of other dyes, partly and are used as dyes themselves. At the same time, they can be obtained directly on the fiber if the original dye is combined in the presence of alkaline reducing agents, such as hydrosulfite or grape sugar, with a highly soluble in water) alkylating agent. At the same time, a reduction product is first formed on the fiber, corresponding to the original dye, which, then, due to the alcohol present at the same time, turns into an insoluble alkylated product, which is so fast and complete that no noticeable separation of the dye from the fiber is observed.

In this way, blue, brown-gray to black dyes, the durability of which, in particular, the stability with respect to chlorine and alkali, in comparison with the original dyes, are significantly increased.

Example 1. - A cube is prepared, when heated, from 10 kgr of a brown-red dye, 20 kgr of hydrosulfite, 40 kgr of alkali with a strength of 40 ° Be and 250 l of water. The clear blue-violet solution in the refluxed vat is added gradually at 50 ° C, with vigorous stirring - ethyl bromide before the procedure, until the sample content of the vat after filtration is colorless. The resulting ethyl product, suspended in a liquid in the form of fine blue flakes, is then expelled by a conventional filtration method. In the dry state, it is a dark blue powder, insoluble in water, alkalis, and acids. Crystallizes from organic solvents. So-crystallization from chlorobenzene gives green-violet shiny needles, the melting point of which lies above 300 °. The compound is soluble. In monohydrate with a blue color, which transforms to brown when heated.

If benzyl chloride is used instead of ethyl bromide, then with the same treatment a similar dark blue compound is obtained which is soluble in. Manog Drate, green brown in color and not crystalline without decomposition from chlorobenzene or nitrobenzene.

Example 2.-The cube prepared according to Example 1 was added with vigorous stirring and at a temperature of about 30 ° C ethyl chloroacetate to ionic release of the dye. The compound isolated in the usual way, crystallized from monochloride) benzene, forms small black-violet cristadles, dot

melting of which lies about 240 °. The color of the solution in monohydrate is blue, and after heating it is green.

Under the same conditions as with chloro-acetic acid ester, with monochloro-acetic acid, a corresponding compound is obtained, and the reaction temperature is advisable to be increased to 50 ° -60 °. Filter the selection in; as a sodium salt compound and washed with a solution of cooking, oh salt. After drying, it is a black powder, easily soluble in hot water with violet color and falling out of acidic solutions in blue flakes.

The solution in the monohydrate is colored blue, turning into green when heated. In a weakly acid bath, the wool is colored a greyish-blue color.

Example S.-If, replace the dye used in Example 1 with an olive-green dye (commercially sold in Grento Olive G), prepared in Example 2 from anthracene and sulfur, - that is, under the same conditions of work, black a powder that does not dissolve in common organic solvents and does not melt at 300 °. The color of the solution in monohydrate is olive.

Similar compounds are obtained by using dyes that are marketed under the name: hydrolysis (and hydronic brown O.

To obtain an alkylated derivative on a fiber, proceed as follows. I

Example 4.-First, all cotton paper is stained in the usual manner in a cube with 5-10 / brown / dye. Then prepare a bath of 2-3 cu. see sodium alkali with a strength of 40 ° Be, 1 | -2 g of hydrosulfite, in powder form, and from 4 to 10 g of tremethyl-a-naphthylammonium chloride per liter of liquid, put colored cotton paper / hot or heated to a boiling bath, withstand from 20 to 30 minutes at the same temperature, washed and dried. I thus; The reported color is now already painted in color and has strong properties.

Instead of trimethyl-anapthyl ammonium chloride, other fatty-aromatic quaternary bases can also be substituted: for example, dimethyl benzylphenylammonium chloride (Leukotrop 0) gives a green-blue color. . If other kilating reagents are used, similar color changes occur: for example, at. Using ethylene chlorohydrin produces a blue tone, while a-dichlorohydrin, hydrosulfite and soda lead to more black shades.

The subject of the patent.

The method of producing alkyl derivatives of sulfur-containing vat dyes obtained by heating anthracene with sulfur, characterized in that these dyes are treated with conventional alkylating agents in a substance or on a fiber in the presence of alkaline reducing agents.