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Clean production method of bromamine acid

A clean production, bromo-acid technology, applied in chemical instruments and methods, sulfonic acid preparation, water/sludge/sewage treatment, etc., can solve problems such as low efficiency of BAA preparation from incapable wastewater

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

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Problems solved by technology

[0006] For this reason, the present invention provides a clean production method of bromonic acid to overcome the problem of low production efficiency of BAA caused by the inability to effectively treat the wastewater produced in the process of preparing BAA by solvent method in the prior art

Method used

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  • Clean production method of bromamine acid
  • Clean production method of bromamine acid
  • Clean production method of bromamine acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0123] This embodiment determines the sulfuric acid concentration of brominated material in the BAA preparation process by experiment

[0124] At present, the concentration range of sulfuric acid after dilution of the brominated material in the workshop is 25%-30%. In this embodiment, it is considered to first purify the acid filtration wastewater to remove anthraquinone compounds, and then concentrate dilute sulfuric acid before applying it. For this reason, the diluted acidity should be increased as much as possible to reduce the energy consumption of dilute sulfuric acid concentration. In this embodiment, the quality of the acid filter cake and the composition of the acid filtrate at 30%, 40%, 50%, and 60% diluted acidity are compared successively to determine a reasonable acidity. On the premise of improving the quality of filter cake and reducing the loss of BAA, the diluted acidity should be increased as much as possible.

[0125] Table 1, Table 2, and Table 3 are the ...

Embodiment 2

[0137] This embodiment is verified to different dilution acidity

[0138]Comparative experiment: take the same batch of brominated materials in the workshop, and conduct three parallel experiments with diluted acidity of 25%-30% and 40%-45%, respectively, and compare the data of the two diluted acidities. The data are shown in Table 4-Table 5 :

[0139]

[0140] It can be seen from Table 4 that in two different sulfuric acid dilution acidity intervals, the BAA content in the filter cake has little difference, but the BAA content (external standard) in the filtrate has a large difference, and the sulfuric acid acidity is between 25%-30%. The content of BAA in medium (external standard) is 2-4 times of the acidity of sulfuric acid at 40%-45%, so it can be seen that the diluted acidity of sulfuric acid should be controlled between 40%-45%.

[0141]

[0142] As can be seen from Table 5, neutralizing the BAA content in the filter cake, the sulfuric acid diluted acidity betwe...

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Abstract

The invention relates to a clean production method of bromamine acid. The method comprises the following steps: preparing 1-amino anthraquinone-2-sulfonic acid; preparing a sulfuric acid solution of 1-amino anthraquinone-2-sulfonic acid; adjusting the acidity of a sulfuric acid solution of 1-amino anthraquinone-2-sulfonic acid to a preset value, and adding a brominated material to prepare a bromamine acid crude product; standing a bromamine acid crude product to remove redundant o-dichlorobenzene solution; carrying out thermal refining on the bromamine acid solution, and adsorbing organic matters in the solution by using activated carbon after thermal refining; salting out the solution to obtain a solution containing bromamine acid crystals, compressing the solution, and drying the filter cake to obtain bromamine acid. By adjusting the acidity of the sulfuric acid solution of 1-amino anthraquinone-2-sulfonic acid in the BAA preparation process, the isomer 1-amino-4-hydroxy anthraquinone which is difficult to remove can be effectively reduced, the amount of acid chloride wastewater generated in the subsequent process is effectively reduced, and the content of BAA in the prepared BAA filter cake is effectively increased; therefore, the preparation efficiency of the BAA prepared by the method provided by the invention is effectively improved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a clean production method of bromic acid. Background technique [0002] Bromonic acid (BAA) is a red needle-like crystal with the chemical name 1-amino-4-bromoanthraquinone-2-sulfonic acid. Soluble in water, orange-red paste or powder, mainly used for dye intermediates, the production of acid anthraquinone dyes, widely used in the preparation of anthraquinone raw dyes, acid dyes and disperse dyes. At present, there are many kinds of dyes synthesized by bromic acid, and there is a huge demand for this product in domestic and foreign markets. In summary, the role of bromine and the lack of research technology on bromine affect important tributary standards such as the shade of dyes. And the yield level in its preparation process directly affects the unit cost of bromic acid. Therefore, it is of great economic and social value to develop a production method of bromonic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/53C07C303/22C07C303/44C07C303/08C02F1/28C02F101/30C02F103/36
CPCC07C303/22C07C303/44C07C303/08C02F1/283C07C2603/24C02F2101/30C02F2103/36
Inventor 时娇娇李超
Owner YANCHENG OUHUA CHEM IND
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