83-62-5Relevant articles and documents
Sulfonation method for preparing bromamine acid by solvent method
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Paragraph 0017-0025, (2021/07/14)
The invention discloses a sulfonation method for preparing bromamine acid by a solvent method, which comprises the following steps: (1) adding an inert solvent which is 9-13 times of the weight of 1-amino-anthraquinone into a sulfonation reactor, stirring and heating to 75-85 DEG C to completely dissolve the 1-amino-anthraquinone; (2) starting a vacuum system, continuously heating to 70-100 DEG C, and completing dehydration under the vacuum degree of-0.008 Mpa; (3) cooling to 70-75 DEG C, slowly adding chlorosulfonic acid which is 1.2-1.5 times of the mole number of 1-aminoanthraquinone at a uniform speed within 6-10 hours, starting to heat to 75-85 DEG C, and preserving heat after heating; (4) continuously raising the temperature to 110-130 DEG C, and keeping the temperature after raising the temperature; (5) adding 98% concentrated sulfuric acid of which the mole number is 2.75-3.15 times that of the 1-aminoanthraquinone at 110-130 DEG C, and finishing at a uniform speed within 4-6 hours; and (6) cooling to 60-75 DEG C, preserving heat after cooling, and standing for layering separation. The method has the advantages of thorough conversion, high yield, simple operation, clear control process, low energy consumption, low cost, continuous treatment and automatic operation.
Process for synthesizing 1-amino-anthraquinone-2-sulfonic acid through solid-phase method
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Paragraph 0033; 0037; 0041, (2018/07/06)
The invention provides a method for synthesizing 1-amino-anthraquinone-2-sulfonic acid from 1-amino-anthraquinone. The method comprises the following steps: generating a sulfate solid of 1-amino-anthraquinone through reaction of the 1-amino-anthraquinone and sulfuric acid, and then performing transposition on the sulfate solid of the 1-amino-anthraquinone to generate the 1-amino-anthraquinone-2-sulfonic acid. A process of synthesizing the 1-amino-anthraquinone-2-sulfonic acid by a sulfuric acid method is fundamentally improved; the sulfate of the 1-amino-anthraquinone is efficiently subjectedto transposition reaction under a solid-phase condition without a solvent after generated water is removed, so that the reaction yield is high, and no side effects are caused; furthermore, no 1-amino-4-chloroant-2-sulfonic acid is generated, and no wastewater, waste gas and waste residues are generated; an obtained product is further synthesized into bromamine acid, and the purity of the obtainedbromamine acid is close to 100 percent; the quality and the yield of the bromamine acid are both higher than the quality and the yield of bromamine acid synthesized by a chlorosulfonic acid method, afuming sulfuric acid method and a conventional sulfuric acid method.
OPTIMIZATION OF THE OXIDATIVE BROMINATION OF 1-AMINOANTHRAQUINONE-2-SULFONIC ACID
Gerasimov, S. V.,Filimonov, V. D.
, p. 928 - 930 (2007/10/03)
An efficient method of synthesis of 1-amino-4-bromoanthraquinone-2-sulfonic acid using bromination of the corresponding aminoathraquinonesulfonic acid with bromine in the presence of hydrogen peroxide has been proposed.The optimum conditions of synthesis, with a yield of the target product of 68percent, have been found.