SU668617A3 - Solid dyeing preparation - Google Patents

Description

The invention relates to the field of dyeing and finishing production, in particular, to the solid dye preparation used to obtain dyeing solutions. A solid dye preparation containing 45% by weight of a cold water soluble dye or optical bleach containing a group capable of forming a hydrogen bridging bond and 50% by weight of an aprotic polar compound urea 1 is known. The disadvantage of this drug is its low solubility in water (10–20 g / l) with the appropriate solubility of the dye contained in it 4.5–15 g / l. The purpose of the invention - increasing tensile vorimosti preparation in cold water Said object is achieved due to the DD that the aprotic polar compound preparation comprises tetramethyl hexamethylphosphoric triamide or N-methylpyrrolidone dimorfolinomochevinu, dimethylacetamide or dimorfolinokarbonil, at present the following component ratio, wt% : Dye or optical brightener42,7-78 Aprotic polar compound Remaining Other compounds that are used in dye or optical brighteners are: molecules groups capable of forming hydrogen bridges, such Gruppyrovki contain N atoms, which may exist simultaneously with the two atoms in the reaction conditions SRI. These groups include groups. -NHj, -NH, OH, -COOH, -SOjH sulfonamido group, for example, a group and a carbonamido group, where R is hydrogen or an alkyl group with 1-4 C or a phenyl group. Such groups may be contained in the dye or optical bleach molecule in an amount of from one to several. Acidic, metal-active metal complex (1: 1 or 1: 2) or basic dyes “Anionic and cationic optical brighteners can belong to the most diverse classes of compounds, such as, for example, 4,4-bis- (triazinylamino) -style6- 2,2-disulfonic acids; 4,4-bis (1,2,3-triazol-2-yl) -stilben-2, 2-disulfonic acids; 1,3-diphenylpyrazolines; distyryl-4,4-biphenylams and distyryl-1,4-benzenes of the benzo-furan derivative with extension pairing residues in position 2 of the mono- and bis-benzoxazole derivatives; mono- and bis-benzimidazole derivative; stilbenes with heterocyclic substituents in position 4 or 4.4 (preferably stilbenyl-naphthriazolam); monometin-cyaninamg naphthalimides (preferably, with ether substitution at position 4 or 4,5); 4-styryl-4- {2-aryl-1, 2,3-triazol-4-yl-ethynyl) -bI phenyls, as well as to compounds with 1,2,4-oxadiazole residues. Aprotic polar compounds contain fluorine, chlorine, oxygen, sulfur, and nitrogen, with which hydrogen is associated with substances capable of forming hydrogen bridges, for example, a dye with a hydrogen atom becoming the positive end of a dipole, and an electronegative element is negative. in a way. The dye or optical brightener is fused either in solid form or in the form of a cake or aqueous solution with aprotic polar compound, as well as g: other additives, after which it is cooled and the water is separated. The melting point depends on the boiling point of the polar compound and on the melting point. of the resulting adduct and fluctuates within 150-200 C. The alloy is hardened by well-known methods, for example by spraying or scaling. You can also allow the melt to harden and transfer it to a granulate. In terms of their shape and cooling, they are crushed to tiles and balls of a certain weight, suitable for dosing dye. It is advisable to grind the melt into flakes, since they dissolve particularly quickly and easily. It is also possible to obtain a preparation by dissolving optical bleach at elevated temperatures in an organic solvent, for example dimethylformamide, acetone or methyl ethyl ketone, together with an aprotic polar compound and other additives — in this case, the preparation is precipitated with a solution. Thus, the drug was an intermolecular adduct, and dependencies on the number of groups in a lecture capable of forming hydrogen bridges were obtained, for example, Isl or 182 adducts in which 1 dye with the group WHj. is attached to 1 mol of polar compound (Isl adduct). Solid: adducts are characterized in that they contain about 2580% by weight of a dye or optical brightener; 10-75% by weight of an aprotic polar compound. Examples 1-9.43 g (0.10 mol) of the dye of the structural formula I are heated at 200 ° C for 8 min together with 17.9 g (0.10 mol) of hexamethylphosphoric triamide. Upon cooling, the melt barks a crystalline solid (1: 1) preparation (the dye content is 70.5 wt.%; The aprotic polar compound is 29.5 wt.%), The yield is almost 100%, it does not give dust and has a solubility in cold water 30 g / l at 20s. 6 g of the adduct adduct is dissolved in 200 ml of demineralized water for 2 min at 20 s and a solution is obtained, which is then passed through a filter paper to form 50 mg of residue. Proceedings are similar to those described above, but using the dyes and aprotic solvents indicated in the mystic table, using non-earthing preparations of dyes with a high dye content and with very good solubility in water. Example 10. 10.9 g (0.02 mol) of the dye of structural formula II $ Og-HH - (, OH is heated for 30 minutes under reflux together with 4 g (0.02 mol) of dimorpholine urea in 10 ml of dimethylformamide The resulting solution was incubated overnight at room / temperature. The mass that crystallized out was stirred with 10 ml of acetone, filtered, three to four times, dried with acetone, 3-5 ml each time, and dried on air. It is of 73.1% by weight of the superhigh dye of 26.9% hgb by weight of dholorfolinochocheins. instead of dimethylformamide, appropriate amounts of acetone or methyl ketone, with the same treatment, an adduct of the same color is obtained. 5 Example 11. 82.5 g (0.02 mo of the dye of structural formula III is dissolved in an excess of tetramethyl urea at which the solvent is distilled off in vacuo. A non-dusting dye preparation is obtained, consisting of 78% by weight of the above dye and 22% by weight of tetramethylmipol 100 ° C, fusing with 65 g (0.027 mol) of dimorpholino urea. A melting melt in cooling and grinding gives a water-soluble, non-adherent adduct consisting of 48% by weight of the dye and 52% by weight of diurethrinomine urea with 170c dissolved in 10 ml of N-methyl pyrrolidone, after which the excess complexing agent is removed in vacuum. 16 g of a solid, unstained preparation consisting of 57% by weight of the indicated optical bleach and 42.2% by weight of methylpyrrolidone are obtained. For example 15. 27.7 g (0.03 mol of optical bleach 14 at 190 ° C is fused with 20 ml of N-methylpyrrolidone, the melt is allowed to solidify by cooling to. Powder preparation consisting of 57.3 IHF. % optical brightener and 42.7 wt N-methylpyrrolidone, does not give dust and dissolves well in water. Example 16. 50 g of the dye of Example 4 together with 20 g of dimorpholinocarbonyl in 100 ml of water are boiled until completely dissolved. vacuum water. A dry crystalline preparation consisting of 28.6% by weight of dimorpholinocarbonyl and 71.4% by weight of the dye of Example 4 does not give a drink. Example 17. If in the example, instead of a dry dye, a cake of dye containing about 50% of a dry product is used, the same results are achieved without additional addition of water.

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its solubility in cold water (30 g / l 20 C in comparison with 7 g / l at pure dye).

Example 14. 9.24 g (0.01 mol) of optical bleach of structural formula Y 76 chevina with good solubility in cold water (50 g / l with a comparatively 10 g / l with a pure dye). Example 12. 15 g (0.035 mol) of the dye were fused at 210- with 9 g (0.045 mol) of dimorpholino-urea, to form a non-dusty and fast-dissolving adduct in water, consisting of 62.5% by weight of the dye and 37.5% by weight .% dimorpholino urea. Example 13. 50 g (0.085 mol) of the dye of structural formula IY., / L Example 18. KZSg dye cake of example 11 is added 14 g of dimorpholinocarbonyl and 15 ml of water. Water is removed in vacuo. The dry preparation, consisting of a CZ 58.8 wt.% Dye and 41.2 wt.% Dimorpholinocarbonyl, does not produce dust and is much more soluble in cold water than the untreated dry dye (40 g / l at 20 s) and differs from 10 g / l at 20 ° C). Example 19. 100 g of the dye of structural formula YI are fused With 120 g of dimorpholinocarbonyl at. A thin melt is sprayed through a granulating device. A non-dusting adduct (in the form of a granulate) is obtained, consisting of | 45.5% by weight of the specified dye and 54.5% by weight of dimorpholinocarbonyl and possessing very good solubility in cold water (50 g / l at 20 ° C) difference from 10 g / l with pure dye).

Example 20. 1g of the preparation prepared according to Example 4 is dissolved in 100 ml of cold water. Using 10 ml of this solution, a coloring solution (250 ml) with 0.15 ml of 80% acetic acid is obtained

and 1 ml of 10% aqueous UNIVADINE PA - Vnivadin PA In this solution, 5 g of Helank tissue (polyamide) is dyed red.

The solubility of the drug increases at 20 ° C from 10-20 g / l to 30-40 g / l with the corresponding solubility of the dye contained in it 21.1522 -5 g / l.

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Claims (1)

; 2 Claims of the invention A solid dye preparation containing a cold water soluble dye or an optical bleach containing a group, a way to form a hydrogen bridge, and an aprotic polar compound, characterized in that in order to increase the solubility of the drug in cold water As an aprotic polar zinchene, it contains hexame triamide. Continued table I zlt :: one Hexamethylphosphoric acid triamide, tetramethyl or dimorfolinomochevinu, N-methylpyrrolidone, dimethylacetamide or dimorfolinokarbonil, with the following component, wt.%: The dye or optical brightener 42,7-78 aprotic polar soedinenieOstalnoe Sources of information received note in the examination 1, Patent of Germany 2322308, cl. 22a 67/00, 1973.