Improved technique for synthesizing dispersion blue 60

A synthesis process, a technology for disperse blue, applied in the field of improved disperse blue 60 synthesis process improvement, can solve the problems of long condensation reaction time, low reaction activity, long reaction time, etc., and achieves improved equipment utilization, reduced reaction temperature, shortened The effect of the production cycle

Inactive Publication Date: 2008-02-27
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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  • Improved technique for synthesizing dispersion blue 60
  • Improved technique for synthesizing dispersion blue 60
  • Improved technique for synthesizing dispersion blue 60

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 40ml of concentrated sulfuric acid into a 250ml four-necked flask, slowly add 20g of 1,4-diamino-2,3-dicyanoanthraquinone after the temperature is raised, and after the addition, the temperature is raised to 70°C and the reaction is kept for two hours. The end point is detected by the pull plate. Then the temperature was lowered to 40°C, 120ml of water was slowly added dropwise to isolate, and then filtered while hot, and the filter cake was washed with hot water.

[0026] Put the above filter cake into a 250ml four-necked flask, add 120ml of water and stir evenly, then add 6g of sodium hydroxide and 2g of activated carbon, increase the temperature to 100℃ and keep the reaction for one hour, filter while hot, wash the filter residue with hot water, and combine the mother liquor And the washing liquid, in the flask, the temperature is raised to 60℃, and then 10ml of 40% sulfuric acid is slowly added dropwise. After the addition, the temperature is raised to 100℃ and the ...

Embodiment 2

[0029] Using the same feeding ratio and operation method as in Example 1, 80ml γ-ethoxypropylamine was used instead of 80ml γ-methoxypropylamine during condensation. After the same treatment, 25.1g of the product was obtained, with a total yield of 93.4%, proofing The brilliance was determined to be 0.8.

Embodiment 3

[0031] Add 40ml of concentrated sulfuric acid to a 250ml four-necked flask, slowly add 20g of 1,4-diamino-2,3-dicyanoanthraquinone after the temperature is raised, and then heat up to 70°C and keep the reaction for two hours. The pull plate detects the end point Then the temperature was lowered to 40°C, 120ml of water was slowly added dropwise to isolate, and then filtered while hot, and the filter cake was washed with hot water.

[0032] Put the above filter cake into a 250ml four-neck bottle, add 120ml of water and stir evenly, then add 6g of sodium hydroxide, heat up to 100°C and keep the reaction for one hour, filter while hot, wash the filter residue with hot water, combine the mother liquor and lotion In the flask, the temperature is raised to 60°C, and then 10ml of 40% sulfuric acid is slowly added dropwise. After the addition, the temperature is raised to 100°C and the reaction is kept for one hour, filtered while hot, the filter cake is washed with hot water and dried.

...

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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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B5/02
Inventor 尹云
Owner JIANGSU YABANG DYE
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