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Preparation method of bromine ammonia blue

A technology of ammonium bromide and ammonium bromide, which is applied to the preparation of sulfonate, chemical instruments and methods, and anthracene dyes, can solve the problems of reducing the amount of catalyst used, incomplete conversion of bromamine, and reducing biscondensates, etc., to achieve Effects of reducing heavy metal content, increasing yield, and reducing usage

Active Publication Date: 2015-02-04
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The object of the present invention is to propose a kind of preparation method of bromamine blue, to realize bromamine nearly 100 % conversion, no hydrolysis of bromoacidic acid (purple by-product) and debrominated by-products, significantly reducing the generation of bicondensates, significantly increasing the yield of condensation products, reducing the discharge of acid-containing and deep-color wastewater; at the same time, it can also reduce The amount of catalyst used, without using copper powder, reduces the content of heavy metals in condensation products, reduces the content of heavy metals in wastewater, reduces environmental pollution, and reduces production costs

Method used

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  • Preparation method of bromine ammonia blue
  • Preparation method of bromine ammonia blue
  • Preparation method of bromine ammonia blue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Take by weighing 9.20 grams of 2,4,6-trimethyl-3,5-diaminobenzenesulfonic acid (M acid), 8.4 grams of sodium bicarbonate, and 20 milliliters of water, add to the tank equipped with agitator, condenser and thermometer In a container, heat to 80°C with stirring. Weigh respectively 8.08 grams of bromine, 15% mol (based on bromine) of monovalent copper and 1,4,7,10-tetraazacyclododecane-1,3-diene (C 8 h 18 N 4 ) complex aqueous solution. Alternately add solid bromine and monovalent copper complexes into the container within 1 hour, keep the reaction temperature at 80-82°C, and the pH of the reaction system at 9, stir for three hours, keep the reaction temperature at 85-90°C, and stir the reaction , sampling for thin-layer chromatography and liquid chromatography analysis, no bromidine as the reaction end point. In the reaction liquid mixture, there are no hydrolyzed products of bromoacidic acid (purple side) and bicondensates, but there are traces of debrominated produc...

Embodiment 2

[0044] Weigh 23 grams of 2,4,6-trimethyl-3,5-diaminobenzenesulfonic acid (M acid), 26.5 grams of sodium carbonate, and 50 milliliters of water, and add them to a container equipped with a stirrer, a condenser and a thermometer , heated to 80°C with stirring. Weigh respectively 20.2 grams of bromine, 10% mol (based on bromine) of monovalent copper and 1,4,7,10-tetraazacyclododecane-1,3-diene (C 8 h 18 N 4 ) complex aqueous solution. Alternately add solid bromine and monovalent copper complexes into the container within 2.5 hours, keep the reaction temperature at 80-82°C, and the pH of the reaction system at 9, stir for three hours, keep the reaction temperature at 85-90°C, and stir the reaction , sampling for thin-layer chromatography and liquid chromatography analysis, no bromidine as the reaction end point. In the reaction liquid mixture, there are no hydrolyzed products of bromoacidic acid (purple side) and bicondensates, but there are traces of debrominated products.

...

Embodiment 3

[0047] Take by weighing 9.20 grams of 2,4,6-trimethyl-3,5-diaminobenzenesulfonic acid (M acid), 8.4 grams of sodium bicarbonate, and 20 milliliters of water, add to the tank equipped with agitator, condenser and thermometer In a container, heat to 80°C with stirring. Weigh respectively 8.08 grams of bromine, 10% mol (based on bromine) of monovalent copper and 1,4,7,10-tetraazacyclododecane-1,3-diene (C 8 h 18 N 4 ) complex ethanol solution. Alternately add solid bromine and monovalent copper complexes into the container within 1 hour, keep the reaction temperature at 80-82°C, the pH of the reaction system is 9, stir for 2 hours, keep the reaction temperature at 85-90°C, and stir the reaction , sampling for thin-layer chromatography and liquid chromatography analysis, no bromidine as the reaction end point. In the reaction liquid mixture, there are no hydrolyzed products of bromoacidic acid (purple side) and bicondensates, but there are traces of debrominated products.

[...

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Abstract

The invention provides a preparation method of bromine ammonia blue. The preparation method comprises following steps: carrying out a condensation reaction between bromamine acid and 2,4,6-trimethyl-3,5-diaminobenzenesulfonic acid with a catalyst system containing a cuprous complex for catalyzing the reaction and then performing seperation to obtain the product bromine ammonia blue (sodium 1-amino-4-((3-amino-2,4,6-trimethyl-5-sulfonylphenyl)amino)-anthraquinone-2-sulfonate) after the reaction finished. By means of utilization of the catalyst system containing the cuprous complex, usage amounts of cuprous chloride and copper powder can be effectively reduced, thereby reducing the content of heavy metals in a dye product, reducing the content of heavy metals in waste water and reducing environmental pollution and production cost. In addition, the preparation method can avoid generation of a hydrolyzed by-product (a purple by-product) of the bromamine acid, can greatly reduce the generation of a debromination by-product, can significantly reduce the generation of a double-condensation substance, can increase yields of the condensation reaction and the dye product and can reduce discharge amount of waste water containing acids and being high in chroma.

Description

technical field [0001] The invention relates to reactive dye technology, in particular to a preparation method of bromamine blue. Background technique [0002] Bromamine blue (1-amino-4-((3-amino-2,4,6-trimethyl-5-sulfophenyl)amino)-anthraquinone-2-sulfonate sodium) is an acid dye, It is also an important dye intermediate (blue base), mainly used in the production of reactive dyes, such as C.I. reactive blue 49, C.I. reactive blue 50, C.I. reactive blue 74, reactive brilliant blue 103 or reactive blue 166, etc. These reactive dyes are resistant Excellent alkali performance, excellent light fastness and soaping fastness, and good solubility. [0003] The structure of bromidine blue is a compound with general formula I: [0004] [0005] At present, the condensation process of bromic acid and 2,4,6-trimethyl-3,5-diaminobenzenesulfonic acid for the preparation of bromamine blue is as follows: [0006] [0007] The condensation reaction of bromic acid and 2,4,6-trimethy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/34C07C309/53C07C303/32B01J31/22
Inventor 吕荣文高崑玉
Owner DALIAN UNIV OF TECH
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