Supercharge Your Innovation With Domain-Expert AI Agents!

Disperse blue 359 preparation method

A technology of disperse blue and sulfonic acid, applied in chemical instruments and methods, organic dyes, anthracene dyes, etc., can solve problems such as difficult to stabilize product quality, low brilliance of disperse blue 359, great influence on yield, etc.

Active Publication Date: 2014-08-06
JIANGSU DAOBO CHEM
View PDF6 Cites 10 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The original production method is mainly to use 1-aminoanthraquinone as raw material to produce 1-aminoanthraquinone-2 sulfonic acid through sulfonation, then bromide to obtain bromic acid, and then obtain the product through amination and cyanation; but the The method has the deficiencies in the following aspects. First, directly carry out bromination with the product of 1-aminoanthraquinone sulfonation reaction, and the reaction yield is 75%. If an appropriate amount of sodium chloride, potassium chloride or sulfuric acid is added in the bromination Sodium, the reaction yield can only be mentioned to 85%; Secondly, in the condensation reaction of bromic acid and ethylamine, the quality of bromic acid, such as impurity content, solubility in water and the content of insoluble matter, etc. have a great impact on the condensation reaction. The yield has a great influence on the yield; another shortcoming is that the impurities brought in in the bromic acid also enter the product, making it difficult to stabilize the product quality. Overall, the disperse blue 359 brightness obtained is generally low

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Disperse blue 359 preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Synthesis of Step 1 1-aminoanthraquinone-2-sulfonic acid:

[0023] In a 500ml four-neck flask, add 150g DMF and 25g 1-aminoanthraquinone, stir for 30 minutes, raise the temperature to 80°C, and add 14g chlorosulfonic acid dropwise at this temperature. After the dropwise addition was completed, the temperature was raised to 90° C., and the temperature was maintained for 8 hours until the end of the reaction. Cool down to below 70°C, and slowly add 800g of water dropwise. After cooling down to 5°C, the material was suction filtered, the filter cake was washed with hot water at 60°C until neutral, and the filter cake was dried. 34g of 1-aminoanthraquinone-2-sulfonic acid was obtained, the content was 98%, and the yield was 98%.

Embodiment 2

[0025] Synthesis of Step 1 1-aminoanthraquinone-2-sulfonic acid:

[0026] In a 500ml four-neck flask, add 200g DMF and 25g 1-aminoanthraquinone, stir for 30 minutes, raise the temperature to 80°C, and add 17.5g chlorosulfonic acid dropwise at this temperature. After the dropwise addition was completed, the temperature was raised to 95° C., and the temperature was maintained for 8 hours until the end of the reaction. Cool down to below 70°C, and slowly add 800g of water dropwise. After cooling down to 5°C, the material was suction filtered, the filter cake was washed with hot water at 60°C until neutral, and the filter cake was dried. 33.9g of 1-aminoanthraquinone-2-sulfonic acid was obtained, with a content of 98.2% and a yield of 97.9%.

Embodiment 3

[0028] Synthesis of Step 1 1-aminoanthraquinone-2-sulfonic acid:

[0029] In a 500ml four-neck flask, add 250g DMF and 25g 1-aminoanthraquinone, stir for 30 minutes, raise the temperature to 80°C, and add 20g chlorosulfonic acid dropwise at this temperature. After the dropwise addition, the temperature was raised to 100° C., and the temperature was maintained for 8 hours until the end of the reaction. Cool down to below 70°C, and slowly add 800g of water dropwise. After cooling down to 5°C, the material was suction filtered, the filter cake was washed with hot water at 60°C until neutral, and the filter cake was dried. 33.8 g of 1-aminoanthraquinone-2-sulfonic acid was obtained, with a content of 98.5% and a yield of 98%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The present invention discloses a disperse blue 359 preparation method, which comprises four reaction units such as sulfonation, chlorination, amination and cyanation. According to the present invention, the improvements of the process comprise that: DMF is adopted as a solvent so as to substantially reduce the reaction temperature, 1-amino anthraquinone-2-sulfonic acid produced through a reaction of 1-amino anthraquinone and chlorosulfonic acid can be directly driven out from the solvent with water so as to provide the simple process operation and increase the yield by nearly 3% compared with the yield of the original process, and the mature acid DMF wastewater recovery process is provided; in the new process, 1-amino anthraquinone is adopted as the raw material and is subjected to sulfonation to produce 1-amino anthraquinone-2-sulfonic acid, and then chlorination is performed to prepare the 1-amino-4-chloroanthraquinone-2-sulfonic acid, wherein the purity of the 1-amino-4-chloroanthraquinone-2-sulfonic acid is high and the yield is 95% while the maximum yield of bromaminic acid prepared by adopting 1-amino anthraquinone as the raw material and carrying out sulfonation and bromination in the original process is 85%; and the product prepared by carrying out amination and cyanation on 1-amino-4-chloroanthraquinone-2-sulfonic acid has the excellent quality, and the brightness is up to more than 1.0.

Description

technical field [0001] The invention belongs to the technical field of chemical material preparation, and in particular relates to the preparation and process of disperse dye disperse blue 359. Background technique [0002] Disperse Blue 359 (Disperse Blue 359), the chemical name is 1-amino-4 (ethylamino) anthraquinone-2 carbonitrile, it is one of the ternary colors with a wide range of applications, and it is mainly used in inkjet printing and In transfer printing, the use of inkjet printing has changed the traditional printing and dyeing process and played a decisive role in improving the environment in subsequent printing and dyeing. Its molecular formula is C17H13N3O2, and its relative molecular mass is 291.3. The structural formula of Disperse Blue 359 is: [0003] [0004] The original production method is mainly to use 1-aminoanthraquinone as raw material to produce 1-aminoanthraquinone-2 sulfonic acid through sulfonation, then bromide to obtain bromic acid, and ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/28
Inventor 徐松刘学峰郭维成汪港孙中华
Owner JIANGSU DAOBO CHEM
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More