Method for preparing blue reactive dyes

A reactive dye, blue technology, applied in reactive dyes, azo dyes, organic dyes, etc., can solve the problems of insufficient wet rubbing fastness, small sewage discharge, and insufficiently bright color, achieving bright color, thorough reaction, The effect of low production cost

Active Publication Date: 2015-04-29
HUBEI HUALI DYESTUFF INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of blue reactive dyes, through the selection of targeted catalysts and some raw materials to solve the problem that the traditional reactive blue P-3R color is not bright enough, the syn...

Method used

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  • Method for preparing blue reactive dyes
  • Method for preparing blue reactive dyes

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Experimental program
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Embodiment 1

[0032] 1) Primary condensation reaction: heat 100 parts of bromic acid to 80°C, disperse for 2 hours, add 102 parts of M acid solution, and maintain the temperature at 95°C for 12 hours in the presence of 20 parts of catalyst copper sulfate pentahydrate to obtain primary condensation For the end point of chromatographic detection, it is required that HPLC>95%;

[0033] 2) Refining: Cool down the primary condensate to 0-20°C, adjust the pH=1-2 with hydrochloric acid, and then add 8% sodium chloride in total volume to salt out and purify to obtain the refined product;

[0034] 3) Secondary condensation reaction: after dissolving the refined product, react with 90 parts of cyanuric chloride at pH=5.2-5.5, temperature 5-7°C for 4 hours to obtain a secondary condensation liquid;

[0035] 4) Tertiary condensation reaction: Add 90 parts of p-aminobenzenesulfonic acid powder into the secondary condensation liquid, react for 8 hours at a temperature of 45-48°C, pH=6-7, and perform TLC ...

Embodiment 2

[0038] 1) Primary condensation reaction: heat 100 parts of bromic acid to 80°C, disperse for 2 hours, add 104 parts of M acid solution, and maintain the temperature at 93°C for 10 hours in the presence of 22 parts of catalyst ferrous chloride mixture to obtain a Condensate, as the end point of chromatographic detection, requires HPLC>95%;

[0039] 2) Refining: cool down the primary condensate to 0-20°C, adjust the pH=1-2 with hydrochloric acid, and then add 10% of the total volume of sodium chloride to salt out and purify to obtain the refined product;

[0040] 3) Secondary condensation reaction: after dissolving the refined product, react with 92 parts of cyanuric chloride at pH=5.2-5.5, temperature 5-7°C for 6 hours to obtain a secondary condensation liquid;

[0041] 4) Tertiary condensation reaction: Add 93 parts of p-aminobenzenesulfonic acid powder into the secondary condensation liquid, react for 8 hours at a temperature of 45-48°C, pH=6-7, and perform TLC chromatography...

Embodiment 3

[0044] 1) Primary condensation reaction: heat up 100 parts of bromine to 80°C, disperse for 2 hours, add 106 parts of M acid solution, and add 24 parts of the catalyst mixture of copper sulfate pentahydrate and ferrous chloride (the ratio of the two is 1:1) In the case of existence, maintain the temperature at 90°C for 12 hours to obtain a condensate, and do the chromatographic detection end point, requiring HPLC>95%;

[0045] 2) Refining: cool down the primary condensate to 0-20°C, adjust the pH=1-2 with hydrochloric acid, and then add 10% of the total volume of sodium chloride to salt out and purify to obtain the refined product;

[0046] 3) Secondary condensation reaction: dissolve the refined product and react with 93 parts of cyanuric chloride at pH=5.2-5.5, temperature 5-7°C for 4 hours to obtain a secondary condensation liquid;

[0047] 4) Tertiary condensation reaction: Add 93 parts of p-aminobenzenesulfonic acid powder into the secondary condensation liquid, react for...

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Abstract

The invention discloses a method for preparing blue reactive dyes. The method comprises the following steps: (1) primary condensation reaction, to be specific, taking copper sulfate pentahydrate, ferrous chloride or a mixture of copper sulfate pentahydrate and ferrous chloride as a catalyst, and enabling bromamine acid and M acid to be subjected to the condensation reaction; (2) refining, to be specific, refining all primary condensation compounds; (3) secondary condensation reaction, to be specific, enabling the refined compound and cyanuric chloride to react to obtain secondary condensation compounds; (4) ternary condensation reaction, to be specific, enabling the obtained secondary condensation compounds and aminobenzene sulfonic acid to react to obtain ternary condensation compounds, filtering, spray drying and packaging, so as to obtain the product. The method can synthesize a new blue reactive dye and has the advantages that the cycle of reaction is shortened, the reaction yield is increased, the reaction is more thorough, the reaction process is clean and environmentally-friendly, the sewage quantity is less, and the prepared product has bright colors.

Description

technical field [0001] The invention belongs to the field of reactive dye synthesis, and in particular relates to a method for preparing blue reactive dye. Background technique [0002] Reactive printing dyes have the advantages of many varieties, complete chromatograms, bright colors, and good wet rubbing fastness. The printing process is simple, the color paste is convenient to prepare, and the printing effect is good. It is one of the most widely used dye categories at present. Among the blue products, Blue P-3R (C.I Reactive Blue 49) is the most important variety, but at present, due to the low solubility of this dye, the synthetic shade is not bright enough, and the traditional salting-out process is used for production, which has a large amount of pollutant discharge. The yield is low, which is not conducive to environmental protection. [0003] Mao Faming studied the synthesis of Mars blue P-3R (dye and dyeing), and believed that the catalyst, the ratio of bromine an...

Claims

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Application Information

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IPC IPC(8): C09B62/06
Inventor 艾良军崔孟元熊建平何向华朱训杰
Owner HUBEI HUALI DYESTUFF INDAL
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