Bromamine acid sodium salt bromination process

A technology of sodium bromamic acid and bromination, applied in the field of bromination of sodium brominated acid salt, can solve problems such as operational risks and potential safety hazards, high sodium chloramic acid salt, affecting product quality, etc., and reduce by-product chlorine. Production of sodium sulfamate, easy handling effect

Inactive Publication Date: 2020-05-08
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

What this method uses is bromine and 1-amino-2-sulfonated liquid to carry out bromination reaction, and the hydrobromic acid produced by sodium chlorate oxidation reaction, will cause the by-product chlorine sodium salt in bromine sodium salt like this High, affects product quality, a...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a 1000ml four-neck flask, add 800g of 3.5% 1-aminoanthraquinone-2-sulfonated solution, heat up to 30~35℃ under stirring, add 32% liquid alkali to adjust 16g to adjust pH=3~4, then add 48% hydrobromic acid, adjust the pH to 2.0~2.5, and finally, add 22g of the total amount of 48% hydrobromic acid and 18g (0.16mol) of 30% hydrogen peroxide dropwise at the same time to maintain the pH=2.0~2.5, and the temperature is 30~35℃ for reaction 3 Hours, until the sampling liquid chromatography detects that the content of 1-aminoanthraquinone-2-sulfonic acid ≤ 0.5% is the end point. After the end point is reached, add liquid alkali to adjust the pH of the material to 7~8, and after the material is separated, vacuum filter to obtain a crude filter cake. Above-mentioned hydrobromic acid total amount comprises the hydrobromic acid that adds twice before and after.

[0022] Add the above crude product filter cake, add water and raise the temperature to 90~95°C, carry out thermal mel...

Embodiment 2

[0024] In a 1000ml four-necked flask, add 800g of 3.5% 1-aminoanthraquinone-2-sulfonated solution, raise the temperature to 30~35℃ under stirring, then add 22g of 48% hydrobromic acid and 20% Sodium bromate solution 20g (0.027mol) and 2g 30% dilute sulfuric acid, maintain pH = 2.0~2.5, temperature 30~35℃, until the sampling liquid chromatography detection, 1-aminoanthraquinone-2-sulfonic acid content ≤ 0.5% Arrive at the end. After the end point is reached, add liquid alkali to adjust the pH of the material to 7~8, and vacuum filter to obtain a crude filter cake. Above-mentioned hydrobromic acid total amount comprises the hydrobromic acid that adds twice before and after.

[0025] Add water to raise the temperature to 90~95°C for the above crude filter cake, carry out thermal melting → filtration → carbon adsorption → filtration → crystallization → filtration to obtain the high-quality bromine sodium salt, liquid chromatography detection: the purity of bromine sodium salt is ...

Embodiment 3

[0027] In a 1000ml four-neck flask, add 800g (0.1mol) of 3.5% 1-aminoanthraquinone-2-sulfonated solution, stir and cool down to 30~35℃, add 16g of 32% liquid caustic soda, adjust pH=3~ 4. Add 48% hydrobromic acid dropwise to adjust the pH of the material to 2.0~2.5, then add 22g (0.13mol) of 48% hydrobromic acid and 75g (0.1mol) of 10% sodium hypochlorite at the same time to maintain pH=2.0~ 2.5, the temperature is 30~35℃, until the sampling liquid chromatography detects that the content of 1-aminoanthraquinone-2-sulfonic acid ≤ 0.5% is the end point; after the end point is reached, add liquid alkali to adjust the pH of the material to 7~8, and vacuum pump Filter to obtain a crude product filter cake. Above-mentioned hydrobromic acid total amount comprises the hydrobromic acid that adds twice before and after.

[0028] Add the above crude product filter cake, add water and raise the temperature to 90~95℃, carry out thermal melting → filtration → carbon adsorption → filtration...

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PUM

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Abstract

The invention relates to the technical field of dyes, in particular to a bromamine acid sodium salt bromination process which comprises the following steps: carrying out sulfonation reaction on 1-aminoanthraquinone and chlorosulfonic acid in an inert solvent to obtain 1-aminoanthraquinone-2-sulfonic acid; after the sulfonation reaction is finished, diluting the liquid with water, performing standing treatment for layering to remove an inert solvent layer, and recycling the solvent by a distillation kettle; pumping an aqueous solution of the sulfonation liquid into a bromination kettle to be subjected to bromination reaction with hydrobromic acid and an oxidizing agent; and alkalizing, filtering and refining the bromination reaction product to obtain the high-quality bromaminic acid sodiumsalt. The invention provides the bromination reaction process of bromamine acid sodium salt, wherein the hydrobromic acid and an oxidizing agent which are low in price and easy to obtain are selected;the reaction temperature is controlled at 30-35 DEG C, the brominated product is filtered and refined to obtain high-quality bromamine acid sodium salt, the generation of byproduct sodium chloramineis reduced, the purity is improved by 0.1-0.3% and reaches 99.6% or above compared with the prior art, and the generated wastewater is also easy to treat. The method is a new safe, green and environment-friendly production process.

Description

technical field [0001] The invention relates to the technical field of dyes, in particular to a bromination process of bromine sodium salt. Background technique [0002] Bromine sodium salt is an important dye intermediate, mainly used in the production of disperse, acidic, reactive and other important dyes. [0003] The Chinese invention patent with the publication number CN106565547A discloses a preparation method and solvent recovery method of bromine sodium salt and its intermediate, specifically disclosing the material layer of 1-aminoanthraquinone-2-sulfonic acid and sulfuric acid and bromine The bromination reaction is carried out with mixing to obtain bromic acid sodium salt. What this method uses is bromine and 1-amino-2-sulfonated liquid to carry out bromination reaction, and the hydrobromic acid produced by sodium chlorate oxidation reaction, will cause the by-product chlorine sodium salt in bromine sodium salt like this High, affects product quality, and becaus...

Claims

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Application Information

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IPC IPC(8): C07C303/08C07C303/22C07C303/32C07C309/53
CPCC07C303/08C07C303/22C07C303/32C07C309/53
Inventor 侯保元汤学斌祝新护
Owner JIANGSU YABANG DYE
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