DE118701C - - Google Patents

Description

IMPERIAL

PATENT OFFICE.

Since in 1873 by croissant and Bretonniere discovered the Cachou de Laval, which is represented in the way It was said that all sorts of organic residues of an indefinite nature, preferably belonging to the fatty series, were heated with alkaline sulfur are only organic in British patent specification 1838 from 1880 Residues, which also include fats, from suitable exposure to baking soda and Spencemetall have been used to represent sulfur dyes. Try to use the Representation of sulfur dyes from bodies of the fat series have been made too led to a rather unexpected fact that fatty acids, especially unsaturated, their salts and esters, under certain conditions, add sulfur-containing 1 dyes are able to deliver that differ from both the Cachou de Laval and those of the British patent specification 1838 and 1880 are very different.

A major novelty of the present invention is the use of soda and Sulfur with partial or complete omission of caustic soda instead of, as hitherto in Sulfur dyes common to the melt using. Sulfur alkalis or from Sulfur and baking soda. A similar procedure was not known up to now.

Those compounds of the fatty series which seem to give the best results are the fatty acids which contain one or more double bonds, i.e. unsaturated fatty acids such as oleic acid C ₁₃ H ₃₄ O ₂ , linoleic acid C ₁₈ Ti ₃₂ O ₂ , castor oleic acid C ₁₈ H _M O ₃ , elaidic acid C ₁₈ H _M O ₂ , as well as those fats, oils or fatty acid derivatives which are capable of supplying unsaturated fatty acids by saponification or by heating with alkaline sulfur. The so-called Turkish red oils, made from castor and olive oil, have also proven to be a suitable material. Pure saturated fatty acids also give direct coloring, but these are mostly less valuable than those derived from unsaturated compounds.

The sulfur dyes obtained from the above-mentioned substances are amorphous, black or gray-black, easily powdered, friable substances. When heated, they swell to 360 to 370 ^° C. and leave a porous, light mass that is almost insoluble in water but is absorbed by sodium sulphide solutions with a brownish yellow color. The new dyes are insoluble in all organic solvents, easily soluble in water, and all the better if a little sodium sulfide is added.

The solutions themselves are bottle- to blue-green or even pure blue in color; even in the latter case, however, brown to brown-black nuances arise on cotton. the end In the solution of the dyes, the acids completely precipitate the coloring components Precipitates are insoluble in all common solvents, even strong ones They are only partially dissolved again in alkalis.

It is very difficult to obtain the coloring matter from the products obtained directly from the oven to be isolated in a more or less pure state, since the dyes are easily decomposed and the precipitated dyes are difficult to filter and redissolve. It is but by repeated precipitation with acids and dissolving in alkaline sulfur and in Sodium hydroxide solution has succeeded in isolating a small amount of a dye, which is a brown-yellow, is an amorphous powder, which is wonderfully cornflower blue in color in diluted sodium sulphide or dissolves soda solutions. The solution is diluted on the addition of Acids fuchsin-red and then separates the dye in flakes. The blue solution slowly oxidizes and takes first a red and finally brown color under Divorce of the dye at.

The new dyes differ from the Cachou de Laval in that they have a somewhat lower resistance to light and chlorine, as well as their greater coloring power and their behavior towards oxidizing agents iron (basic ferric sulfate) of 2 to 3 ⁰ B., of ferric chloride, nitric acid, short of weak oxidizing agents in a reddish to yellowish vivid brown over, similar is the dyeings obtained by natural cachou, the nuance of the cachou de Laval other hand, by this Treatment changed only slightly.

The red-brown colorations obtained by oxidizing agents are obtained by boiling with diluted sulphurous sodium, black-green like the cotton which comes from the dyebath is taken out, and slowly oxidize in the air to a black-brown color.

The fastness to soap, alkalis and diluted acids, as well as direct dyeing as well as that formed after treatment with metal salt solutions is excellent.

The dyes mentioned apparently do not form a uniform product, but rather consist of a mixture of analogous compounds, which are z. B. can be distinguished from one another by the fact that in water they sometimes dissolve with a green, sometimes with a blue color. Small changes in the method of representation often result in significant differences in the finished product. B. prolonged or shorter heating, too great fluctuations in temperature, even the quantity of the mass to be heated causes which can lead to various end products. Is dissolved, for example, the product that is produced from 1 part of castor oil fatty acid, 2 parts of sulfur and 2 parts of soda by 10 to 12stündiges heating to 280 ^0, in water, one obtains an olive-green solution is heated, however, when displaying the mass of more than 300 ⁰ , the solution is a nice bottle green, while it turns into pure blue if it is heated too intensely for a long time. With these color changes, a different solubility in water is connected, by the product, which was heated at 260 ^0, bad, DAS ¹ one who, obtained at 330 ⁰ dissolves completely in water. The product, which is heated above 330 °, gives a blue solution, but leaves behind a considerable insoluble residue; the dye itself is of no importance on account of its poor coloring power.

As an example of the representation of some of these dyes, the following are cited:

I.

5 kg Turkish red oil (oil percentage),
12 "sodium carbonate,

10

Sulfur.

II.

10 kg castor oil soap,
18.5 "sodium carbonate,
20 ,, sulfur.

kg III. IO saponified linseed oil, 21.5 35 Sodium, ^J 9 Sulfur. kg IV. IO Sodium stearate, 25th Sodium, 20th Sulfur.

The mixture is first heated with the addition of about 1 to 1Y ₂ times as much water as the amount of soda used and with constant stirring until the mass becomes thick, then poured into cast iron pots and heated further from 250 ⁰ to 320 to 330 ⁰ C.

You can also start directly from the oils or fats in question by saponifying them with the required amount of sodium hydroxide solution, mixing the reaction product directly with sodium carbonate and sulfur and ^{heating in the oven at 320 to 330 °} C .; the existing

Glycerin does not seem to have any effect on the end result. Or you can also use a mixture of OeI or Up to dickteigiger texture under stirring and then further heated fat, sulfur, sodium carbonate, and water, in little pots on 250 to 320 ^0th Good results are obtained according to the example

V. ■

10 kg pork fat,
20 "sulfur,

2 "solid baking soda,
25 "soda,

40

Water.

In all the examples given, hydrogen sulfide and carbonic acid are released when heated and some sulfur along with small amounts of volatile organic compounds. That finished product forms a black, porous, homogeneous mass that is easily soluble in water, which can be crushed and powdered with ease and used directly for dyeing can be.

The dyes that are obtained according to the various examples given, 'distinguish differ little in their properties despite the difference in the starting materials from each other. They all dye cotton with the addition of table salt in black-brown Tones that differ more in depth than in the type of color.

The specified proportions, the duration and the temperature can be within vary within certain limits, however the figures quoted seem to be quite the most favorable conditions for the ones mentioned To represent fatty acid derivatives.

Claims (1)

Patent claim: Process for the preparation of brown to black-brown direct cotton dyes, consisting in the fact that higher fatty acids, in particular unsaturated fatty acids, their alkali salts and their esters, also Turkish red oils with sulfur and alkali carbonates !! be heated at temperatures up to 330 ^{0 C.}