DE2712656A1 - DYE PREPARATIONS - Google Patents

Description

Bayer Aktiengesellschaft 2712656

-A-

Zentralberetch patents, trademarks and licenses

5090 Leverkusen. 3-layer work

K / Bch

Dye preparations

The invention relates to a process for the production of preparations which are easily dispersible in organic media of water-insoluble dyes sublimable at 100-230 ^. The process is characterized in that the moist press cake obtained during production or the aqueous dispersion of the dye with a solution of a resin in an organic solvent, optionally in Presence of surfactants, mixed without fine division and then the mixture converted into dry form. in the generally this is done by evaporation. In the case of water-miscible solvents, the mixture can also g ^ f. after adding V / ater from ~ esaug-c and then dried. The organic solvent must be chosen so that it with good solubility for the resin, the dye dissolves little.

Resin wherein the solvent is selected so that it forms an azeotrope with water having a boiling point preferably below 100 ⁰ C is preferably dissolved in a water-immiscible solvent. Such solvents are generally known and listed as aqueous azeotrope formers in the Handbook of Chemistry and Physics, 5-6, 1975-1976. For example, benzene, chlorobenzene, m-xylene and toluene

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Called butyl acetate.

The resins used are natural and synthetic condensation resins, resins with a decisive rosin content, hydrogenated Rosin resins, oil-free alkyd resins, maleinate resins, ketone resins, Phenolic resins, chlorinated rubber resins, cellulose esters and ethers and others in the paint and printing ink industry Common, natural or synthetic resins (see Karsten, Lackrohstofftabellen, Verlag R. Vincentz, Hanover (1967)) in question. Cellulose ethers such as ethyl cellulose are preferred used.

The dye preparations according to the invention can be nonionic, contain anionic or cationic surfactants.

Ethylene oxide or propylene oxide adducts with 3 to 50 mol are preferably used as non-icnogenic dispersants Ethylene oxide or propylene oxide on alcohols, alkylphenols, carboxylic acids or amines (see Schönfeldt, Surface active Addition products of ethylene oxide, pp. 18 to 57 (1959)) are used.

Examples of anionic surfactants include:

Sulphated alkylene oxide adducts, sulphated partially esterified polyhydric alcohols, alkyl sulfonates, sodium dialkyl sulfosuccinates, Alkylbenzenesulfonates, condensation products of naphthalenesulfonic acids and formaldehyde, ligninsulfonates and oxylignosulfonates and condensation products from ditolyl ether, formaldehyde and sulfuric acid, or condensation products from m-cresol, 2 naphthol-6-sulfonic acid, Formaldehyde and sodium sulfite.

Suitable cationic surfactants are long-chain ammonium compounds of the zephyrole type.

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Suitable dyes for the production of the preparation according to the invention are:

Disperse dyes of the most diverse classes of dyes and brighteners, especially compounds of the azo and anthraquinone series. Particularly preferred dyes are in the range 160-220 ⁰ C sublimating dyes such as are customarily used in the transfer printing (. See for example GB-PS 1,221,126). Sublimable carbinol bases and carbinol base derivatives (especially ethers) of cationic dyes are also suitable (cf. German Offenlegungsschrift 2,323,538, 2,324,017, 2,325,154 and 2,325,155).

The preparations of the invention contain 30-95%, preferably 45-75 f> dye, 5-70%, preferably 10-50% resin and 0-20 <% surfactant.

In the case of the preferred azeotropic drying, the process is carried out in such a way that press cake (or suspension), if appropriate Dispersant and a solution of resin in an azeotrope former in a suitable aggregate without comminution mixes and the azeotropic mixture and then any excess solvent is distilled off.

In the case of non-azeotrope-forming solvents, water and solvent are distilled off one after the other.

Suitable units are, for example, paddle dryers, thin-film contact dryers or similar devices. Preferred the distillation is carried out in vacuo (P = 10-20 Torr). From the distillate, the organic solvents are recovered and recycled.

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In the case of water-soluble solvents, the resin j also add the solution to an aqueous dispersion which, I

optionally after adding water, it contains enough water for the resin to be insoluble in aqueous solutions
precipitates on the dye surface. Then the
Sucked off the mixture and dried the press cake.

The dry obtained by the method according to the invention ;

Dye preparations can be easily stirred in \

process in organic media into printing inks. Comparison- [ The known preparations are those according to the invention

Preparations due to the better and easier fine distribution ^: as well as superior due to their lower production costs.

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ORIGINAL INSPECTED

example 1

19Og of a water-moist press cake (approx. 30%) of the dye Disperse Yellow 3, (CI. 11855), 15 g of a dispersant the formula

and 100 g of water are homogenized with a high-speed stirrer. A solution of 25 g of ethyl cellulose is added to this mixture N 4 added to 400 g of chlorobenzene. Water and solvent are distilled off in a paddle dryer at a pressure of 20 Torr. The resulting dry dye formation is then ground to a powder, which, for example excellent for the production of gravure printing inks for printing auxiliary carriers for transfer printing.

Example 2

200 g of a finely divided aqueous dispersion (about 30%) des Dye Disperse Red 60 (CI. 60756) and 15 g of the dispersant used in Example 1 are homogenized. A solution of 25 g of ethyl cellulose N 4 in 400 g of chlorobenzene is added to this dispersion. Water and solvents are distilled off in a paddle dryer at a pressure of <v 20 Torr. The resulting dry dye formation is then ground to a »powder.

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Example 3

200 g of a finely divided aqueous dispersion (30? Ig) of i-hydroxy ^ -p-toluidino-anthraquinone and 15 g of the in
Example 1 used dispersants are homogenized. A solution of 25 g of ethyl cellulose N 4 in 400 g of chlorobenzene is added to this dispersion. Water and solvent are distilled off in a paddle dryer at a pressure of A / 20 Torr. The resulting dry dye formation is then ground to a powder.

Example 4

220 g press cake (30 # ig) of the dye Disperse Yellow 3 10 g of the dispersant used in Example 1 and 100 g of water are homogenized with a high-speed stirrer. A solution of 30 g of ethyl cellulose N 4 in 300 ml of methanol is added to this mixture. Water and solvents are in the paddle dryer at a pressure of / V 20 Torr distilled off. The resulting dry dye formation is then ground to a powder.

Example 5

215 g of the aqueous dispersion (dye + dispersant) used in Example 2 are mixed with a solution
ron 25 g of ethyl cellulose mixed in methanol with stirring. Then it is diluted with water until ethyl cellulose has precipitated quantitatively. It is suctioned off, the press cake is dried and ground to a powder.

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Example β

19Og of a finely divided aqueous dispersion (approx. of the dye of 1, 4-dimethylaininoanthraquinone are with 10 g of the dispersant used in Example 1 were stirred up. A solution of 30 g of ethyl cellulose is added to this dispersion given in 400 g of chlorobenzene. Water and solvent are in the paddle dryer at a pressure of / v 20 torr distilled off. The resulting dry dye formation is then ground to a powder.

By simply stirring into a varnish with a fast running Such powdery dye formulations can be processed into printing inks using laboratory stirrers. Due to the high concentrations of the preparation, such printing inks are excellent for printing on transfer printing paper suitable. After subliming, the result is level, clear color tones with a high level of color strength.

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Claims (5)

2712G56 claims 1) A process for preparing readily dispersible in organic media powdery preparations of 100 - sublinierbaren 23O ⁰ C, water-insoluble dyes, characterized in that the aqueous dispersions of this Farbsxcffe or produced during the manufacture, moist presscake of these dyes with a solution of a resin mixed in an organic solvent and then these mixtures are converted into the dry powdery form in a manner known per se. 2) Method according to claim 1, characterized in that the resins used are cellulose ethers, preferably ethyl cellulose, used. 3) Method according to claim 1, characterized in that surfactants are added before the mixture is dried. 4) Preparations obtained according to claim 1. 5) Use of the preparations according to claim 1 for the production of printing inks for printing auxiliary carriers for transfer printing. Ie A 17 953 - 8 - 809839/0308 ORIGINAL INSPECTED