Preparation method of reactive brilliant blue K-GR intermediate

A technology of reactive brilliant blue and intermediates, which is applied in the preparation of sulfonates, chemical instruments and methods, anthracene dyes, etc., can solve the problems of reducing the amount of catalyst used, incomplete conversion of bromoamino acid, and reducing bicondensate, etc. The effect of reducing heavy metal content, improving yield, and reducing usage

Active Publication Date: 2015-02-04
DALIAN UNIV OF TECH
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Problems solved by technology

[0009] The object of the present invention is to propose a kind of reactive brilliant blue K-GR intermediate for the problems of incomplete bromidine conversion, many by-products and high COD in waste water in the preparation method of the existing reactive brilliant blue K-GR intermediate. The preparation method is to realize nearly 100% conversion of bromoacid, no hydrolysis of bromoacid (purple by-product) and debrominated by-product, significantly reduce the formation of bicondensate, significantly increase the yield of condensation products, reduce acid and chromaticity The discharge of deep wastewater; at the same time, it can also reduce the amount of catalyst used, do not use copper powder, reduce the content of heavy metals in condensation products, reduce the content of heavy metals in wastewater, reduce environmental pollution, and reduce production costs

Method used

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  • Preparation method of reactive brilliant blue K-GR intermediate
  • Preparation method of reactive brilliant blue K-GR intermediate

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Weigh 8.4 grams of sodium 2,4-diaminobenzenesulfonate, 8.4 grams of sodium bicarbonate, and 20 milliliters of water, add them to a container equipped with a stirrer, a condenser and a thermometer, and heat to 80°C while 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, the pH of the reaction system at 9, and stir for 3 hours; raise the reaction temperature to 85-90°C, Stir the reaction, take a sample for thin-layer chromatography and liquid chromatography analysis, and no bromidine is the end point of the reaction. In the reaction liquid mixture, there are no hydrolyzed products of bromoacidic acid (purple side) and bicondensates, but there are traces of debrominated products.

[0043] Cool the a...

Embodiment 2

[0045] Weigh 21 grams of 2,4-diaminobenzenesulfonic acid, 26.5 grams of sodium carbonate, and 50 milliliters of water, add them into a container equipped with a stirrer, a condenser, and a thermometer, and heat to 80°C while 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 78-82°C, the pH of the reaction system at 8-9, stir for 3-5 hours; keep the reaction temperature at 80-90 ℃, stirring 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.

[0046] The above materials we...

Embodiment 3

[0048] Weigh 8.4 g of 2,4-diaminobenzenesulfonic acid, 8.4 g of sodium bicarbonate, and 20 ml of water, add them into a container equipped with a stirrer, a condenser, and a thermometer, and heat to 80°C while 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 75-80°C, the pH of the reaction system at 8, stir for 3-4 hours; keep the reaction temperature at 85-90°C, Stir the reaction, take a sample for thin-layer chromatography and liquid chromatography analysis, and no bromidine is the end point of the reaction. In the reaction liquid mixture, there are no hydrolyzed products of bromoacidic acid (purple side) and bicondensates, but there are traces of debrominated products.

[0049] The above materials were coole...

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Abstract

The invention provides a preparation method of a reactive brilliant blue K-GR intermediate. The preparation method comprises following steps: carrying out a condensation reaction between bromamine acid and 2,4-diaminobenzene sulfonic acid or sodium 2,4-diaminobenzene sulfonate with a catalyst system containing a cuprous complex for catalyzing the reaction to obtain the reactive brilliant blue K-GR intermediate (sodium 1-amino-4-((4-amino-3-sulfonylphenyl)amino)-anthraquinone-2-sulfonate). By means of the preparation method of the reactive brilliant blue K-GR intermediate, 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 reactive brilliant blue K-GR intermediate. Background technique [0002] Reactive brilliant blue K-GR intermediate (1-amino-4-((4-amino-3-sulfonic acid phenyl) amino)-anthraquinone-2-sulfonic acid sodium) is an acid dye, but also an important dye Intermediate (blue base), mainly used in the production of reactive dyes, such as reactive brilliant blue K-GR (C.I. reactive blue 2), C.I. reactive blue 4, C.I. reactive blue 5, etc. These reactive dyes have excellent alkali resistance and excellent Excellent light and soap fastness, and good solubility. [0003] Reactive brilliant blue K-GR intermediate is a compound with general formula I: [0004] [0005] At present, the condensation reaction process of bromic acid and 2,4-diaminobenzenesulfonic acid for the preparation of reactive brilliant blue K-GR intermediate is as follows: [0006] [0007] In the abo...

Claims

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Application Information

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