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Blue reactive dye and preparation method thereof

A reactive dye and dye technology, applied in the field of blue reactive dye and its preparation, can solve the problems of large sewage discharge, unfavorable environmental protection, long process time, etc., and achieve the effects of increased solubility, thorough reaction and high dyeing intensity

Active Publication Date: 2020-04-17
HUBEI COLOR ROOT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the Ullmann reaction of Reactive Blue P-3R, copper salt is generally selected as the catalyst. Although the performance of the dye can meet the needs of pad dyeing and printing, the treatment process of the final product requires salting out and filtration, resulting in long process time and The large amount of sewage discharge is not conducive to environmental protection

Method used

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  • Blue reactive dye and preparation method thereof
  • Blue reactive dye and preparation method thereof
  • Blue reactive dye and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of blue active dye, its molecular structure is as shown in formula (1):

[0027]

[0028] In the consumption of each component of this blue reactive dye, 1 part represents 0.1mol, and its preparation method comprises the following steps:

[0029] S1. Ullmann Condensation: Dissolve and disperse 1 part of bromonic acid in 100ml of water, heat up to 80°C and disperse for 2 hours, add 200ml of 1.2 parts of M acid (3,5-diamino -2,4,6-trimethylbenzenesulfonic acid) clarified solution, then add 0.05 parts of stannous chloride in percent, and react at a temperature of 85°C for 6 hours to obtain a primary condensate, the primary condensate When HPLC>98%, it is used as the end point of reaction; the reaction equation of Ullman reaction is as follows:

[0030]

[0031] S2. Recovery of M acid: cool the primary condensate in step S1 to 0°C, adjust pH=1-1.5 to precipitate crystalline M acid, filter and squeeze the crystals through a filter press, and recover 0.2 parts o...

Embodiment 2

[0038] A kind of blue active dye, its molecular structure is as shown in formula (2):

[0039]

[0040] In the consumption of each component of this blue reactive dye, 1 part represents 0.1mol, and its preparation method comprises the following steps:

[0041] S1. Ullmann condensation: Dissolve and disperse 1 part of bromonic acid in 100ml of water, heat up to 80°C and disperse for 2 hours, add 200ml of 1.2 parts of M acid (3,5-di Amino-2,4,6-trimethylbenzenesulfonic acid) clarified solution, then add 0.05 parts of tin protochloride in percent, react at a temperature of 87°C for 7 hours to obtain a condensate, and use a condensate When the HPLC>98% of the product is used as the reaction end point; the reaction equation of the Ullman reaction is as follows:

[0042]

[0043] S2. Recovery of M acid: cool down the primary condensate in step S1 to 2°C, adjust the pH=1-1.5 to precipitate crystalline M acid, filter through a filter press and squeeze the crystalline M acid, an...

Embodiment 3

[0050] A kind of blue active dye, its molecular structure is as shown in formula (3):

[0051]

[0052] In the consumption of each component of this blue reactive dye, 1 part represents 0.1mol, and its preparation method comprises the following steps:

[0053] S1. Ullmann condensation: Dissolve and disperse 1 part of bromonic acid in 100ml of water, heat up to 80°C and disperse for 2 hours, then add 200ml of 1.2 parts of M acid (3,5- Diamino-2,4,6-trimethylbenzenesulfonic acid) clarified solution, add 0.05 parts of tin protochloride in percent, and react at a temperature of 90°C for 8 hours to obtain a primary condensation product, to obtain a primary condensation When the HPLC>98% of the product is used as the reaction end point; the reaction equation of the Ullman reaction is as follows:

[0054]

[0055] S2. Recover M acid: cool down the primary condensate in step S1 to 4°C, adjust pH=1-1.5 to precipitate crystalline M acid, filter and squeeze crystalline M acid thro...

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Abstract

The invention discloses a blue reactive dye and a preparation method thereof. The molecular structure of the blue reactive dye is represented by one or more of a formula (1), a formula (2) and a formula (3) which are defined in the specification. The preparation method of the blue reactive dye comprises the following steps: S1, Ullmann condensation; S2, M acid recovery; S3, secondary condensationreaction; S4, tertiary condensation reaction; and S5, filtration and drying. The method has the technical effects of bright colored light, high color fastness, low sewage discharge in the production process, cleanness and environmental protection.

Description

technical field [0001] The invention relates to the technical field of fuel preparation and production, in particular to a blue reactive dye and a preparation method thereof. Background technique [0002] Reactive printing dyes have the advantages of many varieties, complete chromatograms, bright colors, good wet rubbing fastness, etc., and the printing process is simple, the preparation of color paste is convenient, and the printing effect is good. It is currently one of the most widely used dye categories. Among the blue products, Blue P-3R (C.I Reactive Blue 49) is the most important variety. [0003] In the traditional reactive blue P-3R production process, the Ullmann reaction is usually used to couple the compound raw materials, and then the target dye structure is formed through a series of reactions. In the Ullmann reaction of Reactive Blue P-3R, copper salt is generally selected as the catalyst. Although the performance of the dye can meet the needs of pad dyeing a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B62/06C09B67/24
CPCC09B62/06C09B67/0072
Inventor 沙振中刘振国祝超王婷曾令新沈巍华王燕
Owner HUBEI COLOR ROOT TECH CO LTD
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