DE697065C - Process for the production of concentrated, water-containing dye preparations - Google Patents

Description

Process for the preparation of concentrated, water-containing Dye preparations -It is known that in the recovery of a large number of Dyes, in particular from the class of pigment dyes, from the aqueous Suspension press cake with a relatively low dry content. Accumulate. It was now found that man ho, chlc # o @ n # centered, water-containing dye preparations can be prepared if one in the preparation of the dyes or their aqueous Suspension before or after separating off the mother liquor is difficult or insoluble in water liquid compounds of the aliphatic or isocyclic series in a single bed Adds amount that is insufficient to break the aqueous suspension and the Water-containing dye separates from the liquid in the usual way. Suitable Compounds are, for example, aliphatic or cyclic hydrocarbons or their substitution products, such as hexane, benzene, chlorobenzene, xylene, chloronaphthalene or fatty oils, or the associated fatty acids, terpene alcohols, esters.

It is not only liquids that come into consideration that are highly volatile but also higher molecular weight compounds such as hydrocarbon oils or fats Oils that are in the finished dye dough or in the one available after drying Powder remain. The method can be used for insoluble or in Wasiser sparingly soluble azo dyes, salts of basic or acidic dyes, inorganic ones Pigments, especially lead compounds, and indigoid or anthraquinone vat dyes. The indicated treatment of the aqueous suspension of the dye is. the A considerable part of the water retained in normal work is separated off. So it is z. B.: from 0.5 kg of a 2r, 85%: paste of the azo dye t-amino-2-nitro-q.-chlorobenzene -r _ r-Acetoacetylami, lio - 2 -chlorben.zol with 25 ccm of hexane as much water separate so that the remaining paste contains 60% dye.

The dye preparations obtainable according to the invention can be used for production of paints and for coloring rubber in bulk.

It is known to convert aqueous dye pastes into oil pigment suspensions. In the known method, oil is gradually added to the aqueous dyestuff paste in a mixer until the aqueous suspension is cracked and, with complete separation of the water, an oil-pigment suspension is formed from which the water can be poured off. In the present process, the additive is used in an amount insufficient to break the aqueous suspension. It was not to be expected that a considerable amount of water could be separated by small amounts of additives. Examples i. 500 parts of a --ooioigen paste of the azo dye i-amino-2-riitro-4-chlorobenzöl -> i-acetoacetylamino-2-chlorobenzene are mixed with 25 CCM hexane in a kneader. After a short time the paste has changed in such a way that a large part of the water can be separated by pressing it in the elbows: the paste obtained in this way contains 600,000 dye.

2. To a suspension of 170 parts of the azo dye i-amino-2-nitro-4-chlorobenzene ->. i-Acetoacetylamino-2-chlorobenzene in 2500 parts of water becomes 2o ccm of xylene given. The color paste obtained after separation is 42o, oig.

3. To 500 parts of an a1.7o% paste of the dye i-amino-2-nitro-4-methylbenzene 25 cc of hexane are added to acetoacetylaminobenzene. After a short time you can Separate a considerable amount of water. The paste is 60%.

4 .. An aqueous suspension of 43.5 parts of i - acetoacetylamino - 2 - chlorobenzene is mixed with 25 ccm of chloronaphthalene and in the presence of sodium acetate in the usual way with a diazo solution of 345 parts of i-amino-2-nitro-4-chlorobenzene combined to form the dye. The resulting color paste shows a dry content of 58.8%. Without the addition of chloronaphthalene, a paste of 28.8% is obtained.

5. 500 parts of the 21.5% paste of the azo dye from diazitized i-Amin0-z-nitro-4-methylbenzene and 2-oxynaphtbalin are mixed with 25 cc of xylene in a kneader -staggered: The uniform paste becomes thinner. After separating the water a paste with a dye content of 51.2% is obtained.

6. 250 parts by weight of a 2oo / o aqueous dough of the disazo dye made from 1 mol of tetrazotized 4,4'-diamino-3,3'-dichlorodiphenyl, coupled with 2 mol of i-phenyl-3-methyl-5-pyrazolone, are intimately mixed with 2.5 parts by weight of a mixture of terpene alcohols, such as those z. B. incurred in the production of camphor. The dough that has become thin is vacuumed off. A filter paste with a dry content of 300 / ö is obtained: 7.493 parts by weight: a 17.2% dough of the monoazo dye from diazitized i-amino-2-methoxy-4-nitrobenzene, coupled with 1- (2,3'-oxynaphthoylamino) - naphthalene, are kneaded with 15 g of linseed oil. The dough that has become thin is vacuumed off. The F xpaste obtained now has a dryness of 25%.

. $ t 350 parts of an 18% aqueous dough of the monoazo dye from diazitized i-amino-2-nitro-4-methylbenzene, coupled with z-oxynaphthalene, are kneaded with i2; 6 g castor oil. The dough that has become thin is sucked off: The filter paste obtained now has a dry content of 28%.

9. iöoog of a 23.7% paste of the azo dye i - amino - 2 - methylbenzene - 5 - carboxylic acid - (2'- 4'-dimethyl) - phenylamide -> 1 - (2 ', 3'-oxynaphthoylamino) - 4 - @ chlarbenzol are treated in a kneader with 95 ccm a` resolution of 2.5 parts paraffin @ svachs in 97.5 parts tetrachloroethane. The preparation obtained after squeezing off the water has a dye content of 71.70 / 0.

36.5 kg of the press cake of the azo dye i-amino-2-nitro-4-methylbenzene -Y acetoacetylaminobenzene (Schultz, Dye Tables, 7th Edition, No. 84) with a dye content of 27.4% processed with 4.4 kg of a gasoline-benzene mixture with a benzene content of 100% in a kneader. After squeezing off the water, a water-containing preparation in powder form with a dye content of 60% is obtained.

i i. i 500 g of an i 8.4% aqueous dough of dye 5, 5 '- dichloro - 6; 6 '- dimethyl-2, 2'-bisthionaplithenindigo (Schultz, color tables; 7th ed .; No. 1354) are in the Werner-Pfleiderer with 10 cc of a gasoline-benzene mixture (10% benzene content) kneaded. After prolonged stirring, they can be squeezed out Separate about 600 ccm of water: The remaining powdery preparation i has a Content of 33.5% dye.

Claims (1)

PATENT CLAIM: Process for the production of highly concentrated, Water-containing dye preparations, characterized in that one in the - Preparation of the dyes or their aqueous suspension before or after separation the mother liquor in water sparingly or insoluble liquid compounds of the aliphatic or isocyclic series of such an amount added to my as to break the: aqueous Suspension is insufficient and the water-containing dye in the usual way separates from the liquid.