Novel bromamine acid synthesis process

A kind of bromine acid and new technology technology, applied in the field of organic synthesis, can solve the problems such as low quality and low yield of bromine acid products

Inactive Publication Date: 2021-04-13
YANCHENG OUHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For this reason, the present invention provides a new process for the synthesis of bromonic acid, which can effectively solve the technical pr

Method used

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  • Novel bromamine acid synthesis process
  • Novel bromamine acid synthesis process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0173] After bromination stratification, do different neutralization pH tests on the brominated material:

[0174] Take the brominated stratified material layer, add alkali to neutralize to PH6-7 and PH=9, heat to boiling, retest the pH, and find that the pH will decrease to varying degrees, add liquid alkali to adjust to the specified value, and cool to 50 ℃, filter, take the filter cake for insoluble matter test, observe whether there is insoluble matter precipitation, and the amount of precipitation; and neutralize the salting-out filtrate at pH6-7 with liquid caustic soda to neutralize the filtrate pH9.35, filter, Observe whether any insoluble matter that has not been completely precipitated is re-precipitated under alkaline conditions.

[0175] in conclusion:

[0176] When neutralizing and adjusting the pH to 6-7, there is a small amount of black insoluble matter in the bromine filter cake;

[0177] When the pH is adjusted to 9, there are more brown-black insoluble matt...

Embodiment 2

[0181] Material test after neutralization and heat refining:

[0182] Test the PH and water insoluble matter of the material after heat refining. The material PH after heat refining is about 4-5. After testing, there is no water insoluble matter. When adding alkali to adjust PH=7, there will be a large amount of insoluble matter; therefore, The insoluble matter always exists in the system, and the insoluble matter is in a dissolved state when the pH is 4-5. When the pH value is controlled, the salting out allows the insoluble matter to remain in the salting out solution.

Embodiment 3

[0184] (1) After activated carbon is refined and blank

[0185] Dissolve about 68g of used activated carbon in 200ml of hot water, add hydrochloric acid, filter, the filtrate is measured at PH=1.6, add liquid caustic soda, and a large amount of black insoluble matter is precipitated; the results show that activated carbon adsorbs more insoluble matter.

[0186] (2) Activated carbon blank test

[0187] Take 30g of fresh activated carbon and put it in 200ml of water. Before adding activated carbon, the pH of the water is 8.05. After adding activated carbon, the pH of the water is 2.7. Add hydrochloric acid, filter, and measure the pH of the filtrate. A small amount of yellow-green insoluble matter; the analysis believes that the trace amount of insoluble matter in the small-scale activated carbon blank test is negligible on the basis of the total volume of 30kg and 5000kg of activated carbon in the workshop;

[0188] The above two groups of experiments concluded that activated ...

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Abstract

The invention relates to a novel bromamine acid synthesis process, which comprises: 1, adding 1-amino anthraquinone as a raw material, adding o-dichlorobenzene, adding chlorosulfonic acid in a dropwise manner, carrying out a sulfonation reaction, after reaching sulfonation reaction end point, adding sulfuric acid, adding sodium bromide and sodium bromate, and carrying out a bromination reaction to obtain a reaction product; carrying out bromination layering in a layering device after reaching the bromination reaction end point; 2, when a central control module judges that bromination layering is completed, conveying the brominated material into a second reactor, adding liquid caustic soda for a neutralization reaction, and obtaining a bromamine acid filter cake; 3, when the central control module judges that the water-insoluble substances are completely separated out, putting the bromamine acid filter cake into a third reactor, and adding activated carbon to carry out activated carbon thermal refining reaction; 4, sequentially carrying out salting-out, filter pressing and drying on the bromamine acid filter cake subjected to the activated carbon thermal refining reaction to obtain bromamine acid; therefore, the problem that the bromamine acid contains water insoluble substances can be solved, and the quality and yield of the finished product of the bromamine acid are effectively improved.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a new process for synthesizing bromic acid. Background technique [0002] Bromic acid, the chemical name is 1-amino-4-bromo-2-sulfonic acid anthraquinone, which is an important dye intermediate, mainly used in the manufacture of acid anthraquinone dyes such as weak acid brilliant blue GAW, weak acid brilliant blue R, Reactive Brilliant Blue M-BR, Brilliant Blue KN-R, Brilliant Blue K3R and Brilliant Blue KGR, etc. [0003] In the synthesis process of bromic acid, 1-aminoanthraquinone, as an important intermediate, undergoes sulfonation and bromination reactions to finally generate bromic acid. The Chinese patent with publication number 104086430A discloses a synthesis method of 1-aminoanthraquinone, in which anthraquinone and nitric acid are subjected to insufficient nitration reaction in a solvent to obtain 1-nitroanthraquinone, and 1-aminoanthraquinone is obtained through redu...

Claims

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Application Information

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IPC IPC(8): C07C309/53C07C303/22C07C303/44
CPCC07C303/08C07C303/22C07C303/44C07C2603/24C07C309/53
Inventor 时娇娇李超
Owner YANCHENG OUHUA CHEM IND
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