Improved technique for synthesizing dispersion blue 60

Abstract

The invention discloses a modification of synthesizing technique of dispersion blue 60, which comprises the following steps: adopting 1, 4-diamino-2,3-dicyanidic anthraquinone as raw material to hydrolyze in the sulfuric acid as dielectric at 60-90 deg. c to obtain 1, 4-diamino anthraquinone-2,3-dicarboxylic imides to react with sodium hydroxide to generate corresponding sodium salt to dissolve in the water; adding active carbon to adsorb impurity; filtering under heating; adding sulfated closed-loop in the filtrate to produce 1, 4-diamino anthraquinone-2,3-dicarboxylic acid anhydrides; insulating the anhydride in the gamma-methoxy propylamine (or gamma-ethoxy propylamine) dielectric to react 2-3h under 40-50 deg. c to obtain the product.

Description

Technical field [0001] The present invention relates to an improved synthesis process improvement of Disperse Blue 60. Background technique [0002] Disperse Blue 60, also known as Disperse Blue S-GL, Disperse Turquoise Blue GL, Disperse Turquoise Blue S-GL, Disperse Turquoise Blue S-GLR, etc., is an excellent dye for polyester and its blended fabrics. [0003] The original production method uses 1,4-diamino-2,3-dicyanoanthraquinone as raw material and reacts with sulfuric acid to prepare 1,4-diaminoanthraquinone-2,3-dicarboxyimine. Then it is condensed with corresponding amines such as γ-methoxypropylamine or γ-ethoxypropylamine in a solvent to obtain products. For example, US patents 2628963, 2701802, 2753356, etc. have detailed descriptions of its synthesis; but the method has the following There are several shortcomings. Firstly, the reaction activity of 1,4-diaminoanthraquinone-2,3-dicarboxyimine with amines is low, so the condensation reaction time is longer, and the reacti...

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Problems solved by technology

[0003] The original production method is to use 1,4-diamino-2,3-dicyanoanthraquinone as raw material, and react with sulfuric acid to prepare 1,4-diaminoanthraquinone-2,3-dicarboxyimine, Condensation with corresponding amines such as gamma-methoxypropylamine or gamma-ethoxypropylamine etc. in solvent obtains product again, as US Patent No. 2628963, 2701802, 2753356 etc. have detailed instructions to its synthesis; But this method exists following The deficiencies in several aspects are firstly that the reactivity of 1,4-diaminoanthraquinone-2,3-dicarboxyimine and amines is low, so the condensation reaction time is longer, and the reaction needs to be carried out at high temperature, requiring Select high-boiling point solvents and use pressure equipment for production. After the reaction, it must be diluted with alcohols so that the product is separated out. After mixing multiple solvents, it also brings difficulties to its recovery; secondly, due to 1,4-diaminoanthraquinone-2, 3-dicarboxyimine is a water-insoluble substance, which cannot be refined and removed, so the impurities brought in from the raw materials also enter the product, making it difficult to stabilize the quality of the finished product. Overall, the dyes produced are generally low in brightness. In actual production, in order to improve the purity of the intermediate 1,4-diaminoanthraquinone-2,3-dicarboxyimine, a large amount of Sulfuric acid to increase the dissolution of impurities, thus also leading to an increase in the amount of spent acid; another disadvantage is that the product yield is not high due to its low reactivity

In order to improve its reactivity, someone changed 1,4-diaminoanthraquinone-2,3-dicarboxyimine into 1,4-diaminoanthraquinone-2,3-dicarboxylic acid anhydride, such as US Patent 2770625, Japan Patent Zhao 40-4222, etc., after conversion, its condensation temperature has been greatly reduced, and the yield has also been significantly improved, but because the process has not been refined, the resulting product quality is still relatively poor, and the dye brightness has not been fundamentally improved. The above method Alcohols are used as the reaction medium during condensation, which affects the reaction speed, so the reaction time is longer

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