Method for preparing disperse red

A technology for disperse red and preparation steps, which is applied in the field of preparation of disperse dyes, can solve the problems of complicated process, harsh process conditions, and obstacles to the large-scale use of dispersants, and achieve the effect of simple process and high yield

Inactive Publication Date: 2013-02-27
江苏德旺数码科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the synthesis process in the market is difficult to industrialized production due to the complex process or harsh process conditions, which hinders the large-scale use of this type of dispersant

Method used

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  • Method for preparing disperse red
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  • Method for preparing disperse red

Examples

Experimental program
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Effect test

Embodiment 1

[0018] 1) Preparation of 1-amino-2-(4ˊ-chlorosulfonyl)phenoxy-4-hydroxyanthraquinone: In the reactor, add 10mol of chlorosulfonic acid, cool to 0~5℃, add 1mol of 1-Amino-2-phenoxy-4-hydroxyanthraquinone is added to the process control temperature of 0~5℃, then the temperature is increased to 42~45℃, and the reaction is stirred at this temperature for 1.5~2h. The reaction is monitored by HPLC. -Amino-2-phenoxy-4-hydroxyanthraquinone is consumed, then 1.1 mol of thionyl chloride is added, and the reaction is continued at 42~45°C for 1~1.5h. The reaction is monitored by HPLC. When the intermediate disappears, the reaction Cool the liquid to 0~5℃, then add 0~5℃ water to the reaction liquid, keep 0~5℃ and stir for 5~8min, filter, wash with water and press dry to obtain 1-amino-2-(4'-chlorosulfonate Acyl) phenoxy-4-hydroxyanthraquinone wet product;

[0019] 2) Preparation of l-amino-2-[4'-(3-ethoxypropylaminosulfonyl)phenoxy]-4-hydroxyanthraquinone: add water, solvent and step 1) to t...

Embodiment 2

[0021] 1) Preparation of 1-amino-2-(4ˊ-chlorosulfonyl)phenoxy-4-hydroxyanthraquinone: Add 11.5mol of chlorosulfonic acid to the reactor, cool to 0~5℃, add 1mol under stirring The 1-amino-2-phenoxy-4-hydroxyanthraquinone was added to the process control temperature of 0~5℃, then the temperature was raised to 42~45℃, the reaction was stirred at this temperature for 1.5~2h, and the reaction was monitored by HPLC. After the consumption of 1-amino-2-phenoxy-4-hydroxyanthraquinone is complete, add 1 mol of thionyl chloride and continue the reaction at 42~45°C for 1~1.5h. HPLC monitors the reaction. When the intermediate disappears, the reaction Cool the liquid to 0~5℃, then add 0~5℃ water to the reaction liquid, keep 0~5℃ and stir for 5~8min, filter, wash with water and press dry to obtain 1-amino-2-(4'-chlorosulfonate Acyl) phenoxy-4-hydroxyanthraquinone wet product;

[0022] 2) Preparation of l-amino-2-[4'-(3-ethoxypropylaminosulfonyl)phenoxy]-4-hydroxyanthraquinone: add water, solv...

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Abstract

The invention discloses a method for preparing disperse red. The preparation steps include preparing to obtain 1-amino-2-(4'-sulfonyl chloride) phenoxy-4-hydroxy-anthraquinone, and subjecting the intermediate to reacting with 3-ethyoxypropylamine to obtain 1-amino-2-<4'-(3-ethyoxypropylamine sulfonyl) phenoxy>-4-hydroxy-anthraquinone. The method for preparing the disperse red has the advantages that the process is simple, the yield is high, the total yield is larger than or equal to 95%, the finished product purity is larger than or equal to 99.8%, and the method can meet the requirements of industrial production.

Description

Technical field [0001] The invention relates to the field of preparation of disperse dyes, in particular to a preparation method of disperse red. Background technique [0002] 1-Amino-2-[4-(3-ethoxypropylaminosulfonyl)phenoxy]-4-hydroxyanthraquinone is also known as Disperse Red P-BEL, its structural formula is: [0003] [0004] That is, C.I. Disperse Red 92 is one of the important varieties of anthraquinone disperse dyes. It is suitable for dyeing and printing of polyester and blended fabrics, as well as for dyeing cellulose acetate and nylon. C.I. Disperse Red 92 original dye is a product obtained by chlorosulfonation and aminating condensation of 1-amino-2-phenoxy 4-hydroxyanthraquinone (C.I. Disperse Red 60). Yang Chuanxi and others reported the green synthesis process of 1-amino-2-bromo-4-hydroxyanthraquinone, and the successful research and development of CI Disperse Red 60 improved processes such as Mitsui Togaki Corporation of Japan, which created favorable conditions for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/54
Inventor 杨泽辉何明华钱益民黄祥保
Owner 江苏德旺数码科技有限公司
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