A kind of synthetic method of disperse blue 54

A synthesis method and technology of disperse blue, applied in chemical instruments and methods, anthracene dyes, organic dyes, etc., can solve the problems of unbalanced dinitroanthraquinone, excess dinitroanthraquinone, etc., and achieve easy access to raw materials and production The effect of cost reduction

Active Publication Date: 2021-11-12
JIUJIANG FUDA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As the market demand for disperse blue 77 increases, it will also lead to an imbalance of 1,5(1,8)-dinitroanthraquinone, that is, the problem of excess 1,5-dinitroanthraquinone

Method used

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  • A kind of synthetic method of disperse blue 54

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] The present embodiment provides a kind of synthetic method of disperse blue 54, comprises the steps:

[0063] a. add the mixed solution of 100 milliliters of aniline and 400 milliliters of toluene in reaction vessel;

[0064] b. Start stirring, add dihydroxy dinitroanthraquinone in 1-2 hours, keep the molar ratio of dihydroxy dinitroanthraquinone to aniline at 1:4;

[0065] c. After adding, heat up to 100°C in 1-2 hours, then heat up to 125°C in 2-3 hours, and keep warm for 6 hours;

[0066] d. During the heating and heat preservation process, collect the organic solvent fraction, let it stand for stratification, let off the water layer, and recycle the organic solvent for mechanical use;

[0067] e. Cool down to 70°C;

[0068] f. After the above condensation reaction, the mixture of dihydroxy dinitroanthraquinone, aniline and toluene is cooled to 70°C and then put into a crystallization container, methanol is added as a crystallization solvent, and the temperature is...

Embodiment 2

[0075] The present embodiment provides a kind of synthetic method of disperse blue 54, comprises the steps:

[0076] A. add the mixed solution of 150 milliliters of aniline and 350 milliliters of xylenes in reaction vessel;

[0077] b. Watch the stirring, add dihydroxy dinitroanthraquinone in 1-2 hours, keep the molar ratio of aniline and dihydroxy dinitroanthraquinone to aniline at 1:6;

[0078] c. After adding, heat up to 105°C in 1-2 hours, then heat up to 140°C in 2-3 hours, and keep warm for 3 hours;

[0079] d. During the heating and heat preservation process, collect the organic solvent fraction, let it stand for stratification, let off the water layer, and recycle the organic solvent for mechanical use;

[0080] e. Cool down to 65°C;

[0081] f. Cool the mixture of dihydroxy dinitroanthraquinone, aniline and toluene after the above condensation reaction to 65° C. and put it into a crystallization container, add ethanol as a crystallization solvent, and keep warm for ...

Embodiment 3

[0088] The present embodiment provides a kind of synthetic method of disperse blue 54, comprises the steps:

[0089] a. add the mixed solution of 250 milliliters of aniline and 250 milliliters of ethylbenzene in reaction vessel;

[0090] b. Watch the stirring, add dihydroxy dinitroanthraquinone in 1-2 hours, keep the molar ratio of dihydroxy dinitroanthraquinone to aniline at 1:12;

[0091] c. After adding, heat up to 110°C in 1-2 hours, then heat up to 135°C in 2-3 hours, and keep warm for 4 hours;

[0092] d. During the heating and heat preservation process, collect the organic solvent fraction, let it stand for stratification, let off the water layer, and recycle the organic solvent for mechanical use;

[0093] e. Cool down to 60°C;

[0094] f. Cool the mixture of dihydroxy dinitroanthraquinone, aniline and toluene after the above condensation reaction to 60°C and put it into a crystallization container, add methanol as a crystallization solvent, and keep warm for 1 hour ...

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Abstract

The present invention relates to a kind of synthetic method of disperse blue 54, and it comprises the steps: S1: with 1,5-dihydroxy-4,8-dinitroanthraquinone and 1,8-dihydroxy-4,5-dinitroanthraquinone The mixture of anthraquinone and aniline are condensed in an organic solvent with a boiling point of 110-150°C, and part of the organic solvent is evaporated during the reaction; S2: crystallize the material after the condensation reaction is completed; S3: filter and collect the mother liquor The product was recovered and applied mechanically, and the product Disperse Blue 54 was obtained after washing the filter cake. The present invention directly utilizes 1,5-dinitroanthraquinone and 1,8-dinitroanthraquinone mixture as raw material to prepare dihydroxy dinitroanthraquinone (i.e. 1,5-dihydroxy-4,8-di Nitroanthraquinone and 1,8-dihydroxy-4,5-dinitroanthraquinone mixture) is condensed with aniline to synthesize disperse blue 54, a blue dye with high fastness, without the need for 1,8-dinitro Separation and purification of anthraquinone and solution to the problem of excess 1,5-dinitroanthraquinone.

Description

technical field [0001] The invention relates to a synthesis process of a dye, in particular to a synthesis method of disperse blue 54. Background technique [0002] 1,8-Dinitroanthraquinone is an important intermediate for the synthesis of high-grade disperse dyes (such as synthetic disperse blue 77, disperse blue 27, etc.) and medicine, and it can also be used to synthesize 1,8-substituted anthraquinone derivatives. Anthraquinone is dinitrated by mixed acid (sulfuric acid and nitric acid), and then refined with sodium sulfite to obtain a mixture of 1,5-dinitroanthraquinone and 1,8-dinitroanthraquinone (abbreviation: dinitroanthraquinone). In order to synthesize disperse blue 77, the dinitroanthraquinone mixture needs to be separated and purified to obtain high-purity 1,8-dinitroanthraquinone. [0003] At present, the separation methods of 1,5-dinitroanthraquinone and 1,8-dinitroanthraquinone mainly include acid treatment method and solvent method. The acid treatment metho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B1/514
CPCC09B1/514
Inventor 叶世森彭德新张少波高卫斌
Owner JIUJIANG FUDA IND CO LTD
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