Utilization method of bromamine acid byproduct

A technology of by-product, bromidine, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of waste of resources, environment, pollution, etc., and achieve the effect of protecting the environment and saving resources

Pending Publication Date: 2022-04-29
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no report on the utilization of bromidine by-products. It is mainly treated as solid waste incineration, which not only wastes resources but also causes environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Part of the by-products of bromic acid, namely 1-aminoanthraquinone, 1-amino-2-bromoanthraquinone and 1-amino-2,4-dibromoanthraquinone, were brominated, and 4.75g Pure water, then add 99g of sulfuric acid with a concentration of 90% for magnetic stirring, after stirring evenly, add 50g of bromic acid by-products to the sulfuric acid solution for magnetic stirring; heat the four-necked flask to 100°C, and dropwise add 99 % bromine 50g, carry out 8h bromination reaction, add bromine activator sodium hypochlorite 0.28g simultaneously, then keep refluxing after 13h, take a sample and measure 1-amino-2,4-dibromoanthraquinone content is not less than 98%, promptly reaches end point of the reaction.

[0028] Heat the above reaction mixture to 80°C, keep it for 1h, then raise the temperature to 90°C, keep it for 2h, finally raise the temperature to 102°C, keep it for 3.75h for bromine extraction treatment, then add 144g of sulfuric acid with a concentration of 95% and 3.6g of 9...

Embodiment 2

[0031] Part of the by-products of bromic acid, namely 1-aminoanthraquinone, 1-amino-2-bromoanthraquinone and 1-amino-2,4-dibromoanthraquinone, were brominated, and 4.75g Pure water, then add 99g of sulfuric acid with a concentration of 95% and carry out magnetic stirring. After stirring evenly, add 50g of bromic acid by-products to the sulfuric acid solution for magnetic stirring; heat the four-necked flask to 102°C, and dropwise add 99 %bromine 53g, carry out bromination reaction for 8h, add bromine activator hydrogen peroxide 0.09g at the same time, after keeping reflux for 13h, take a sample and measure the content of 1-amino-2,4-dibromoanthraquinone not less than 98%, that is, the reaction is reached end.

[0032] Heat the above reaction mixture to 83°C, keep it for 1h, then raise the temperature to 93°C, keep it for 2h, finally raise the temperature to 103°C, keep it for 3.75h for bromine extraction treatment, then add 144g of sulfuric acid with a concentration of 98% and...

Embodiment 3

[0035] Partial by-products of bromic acid 1-aminoanthraquinone, 1-amino-2-bromoanthraquinone and 1-amino-2,4-dibromoanthraquinone were brominated, and 4.75 g of pure water, then add 99g of sulfuric acid with a concentration of 100% for magnetic stirring, and after stirring evenly, add 50g of the by-product of bromic acid to the sulfuric acid solution for magnetic stirring; heat the four-necked flask to 99°C, and add 99% Bromine 55g, carry out 8h bromination reaction, add bromine activator chlorine and iodine 0.06g simultaneously, after keeping reflux 13h, take a sample and measure 1-amino-2,4-dibromoanthraquinone content is not less than 98%, promptly reaches end point of the reaction.

[0036] Heat the above reaction mixture to 85°C, keep it for 1h, then raise the temperature to 95°C, keep it for 2h, finally raise the temperature to 104°C, keep it for 3.75h for bromine extraction treatment, then add 144g of sulfuric acid with a concentration of 101% and 3.6g of 99% Urotropin...

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PUM

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Abstract

The invention relates to a utilization method of a bromamine acid byproduct, which specifically comprises the following steps: reacting a part of the bromamine acid byproduct with bromine and an activating agent to obtain a reaction mixture containing 1-amino-2, 4-dibromo anthraquinone; carrying out bromine extraction treatment on the reaction mixture under a certain heating procedure, and then adding sulfuric acid and urotropine to carry out hydrolysis reaction, so as to obtain the 1-amino-2-bromo-4-hydroxyanthraquinone. The process can be used for preparing the 1-amino-2-bromine-4-hydroxy anthraquinone from the main by-products, namely the 1-amino anthraquinone, the 1-amino-2-bromo anthraquinone and the 1-amino-2, 4-dibromo anthraquinone. The 1-amino-2-bromine-4-hydroxy anthraquinone can be widely used for synthesizing disperse red 60, disperse red 91, disperse red 191 and the like, the market demand is large, the situation that in the prior art, by-products serve as solid waste to be incinerated can be avoided, and resource saving and environment protection are better facilitated.

Description

technical field [0001] The invention belongs to the field of organic dye synthesis, and in particular relates to a utilization method of bromic acid by-products. Background technique [0002] Bromoacid, whose chemical name is 1-amino-2-sulfonic acid-4-bromoanthraquinone, is a dye intermediate widely used in the synthesis of acid dyes and disperse dyes. At present, there are more than 30 varieties of disperse dyes and acid dyes used for synthesis, and the market demand is large. [0003] There are many synthetic methods of bromic acid, but the current domestic mainstream process still uses 1-aminoanthraquinone as the main raw material, and sulfonates with chlorosulfonic acid or sulfuric acid as the sulfonating agent under the condition of concentrated sulfuric acid or o-dichlorobenzene as the solvent. Then bromide with bromine to obtain the product bromamide. No matter which process is used, the following by-products will be produced: 1-amino-2-bromoanthraquinone, 1-amino-2...

Claims

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Application Information

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IPC IPC(8): C07C221/00C07C225/36
CPCC07C221/00C07C2603/24C07C225/36C07C225/34
Inventor 詹国青周军姬书亮臧君娇盛保安
Owner JIANGSU YABANG DYE
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