- Preparation method for bromamine acid
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The invention discloses a preparation method for bromamine acid. The preparation method comprises the following steps: 1) taking 1-amino anthraquinone as a raw material and reacting with fuming sulfuric acid and sodium sulfate in a solvent, thereby acquiring a reaction liquor containing sulfonating products, wherein temperature of sulfonating reaction is at 100-150 DEG C and reaction time is 3-10h; 2) cooling the reaction liquor to 60-80 DEG C, adding iodine and anti-foaming agent, slowly dropwise adding bromine for 5-8h, and keeping temperature for 2-3h after the ending of dropwise adding; 3)ending bromination reaction, removing excessive bromine through reduced pressure distillation, adding a certain amount of water, cooling to 50-60 DEG C and filtering, thereby acquiring bromamine acidsulfate; 4) placing bromamine acid sulfate into a large amount of water, heating to 70-90 DEG C, adding sodium hydroxide for regulating pH to 8-9, cooling to 20-30 DEG C and performing suction filtration, thereby acquiring the product bromamine acid. The yield of product is 91% and the purity detected through liquid chromatogram is 99%.
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- Preparation process for sodium 1-amino-4-bromoanthraquinone-2-sulfonate
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The invention discloses a preparation process for sodium 1-amino-4-bromoanthraquinone-2-sulfonate. The preparation process comprises the following steps: (1) sulfonation: with 1-aminoanthraquinone as a raw material, copper sulfate as a catalyst and dichloroethane as a solvent, carrying out dehydration, then adding chlorosulfonic acid drop by drop for a sulfonation reaction, adding 98% concentrated sulfuric acid after completion of the reaction, extracting 1-aminoanthraquinone-2-sulfonic acid out, allowing 1-aminoanthraquinone-2-sulfonic acid to enter the concentrated sulfuric acid, separating out an acid phase at a lower layer and subjecting the acid phase to a subsequent reaction; (2) bromination: adding bromine into the concentrated sulfuric acid solution of 1-aminoanthraquinone-2-sulfonic acid drop by drop for a reaction so as to obtain the concentrated sulfuric acid solution of bromoamine acid; (3) dilution: adding water into the concentrated sulfuric acid solution of bromoamine acid for dilution and successively carrying out cooling, crystallization and filtering so as to obtain bromoamine acid; and (4) salt formation: adding water to dissolve bromoamine acid and adding sodium sulfite to obtain bromoamine acid sodium salt. The preparation process provided by the invention can reduce energy consumption during solvent recovery; the utilization rate of bromine in bromination is high; sodium sulfite is used for salt formation, so the amount of impurities is reduced; and product quality is high.
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- Process for separating off 1-amino-4-bromoanthraquinone-2-sulphonic acid
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A process for separating off 1-amino-4-bromoanthraquinone-2-sulphonic acid from the reaction mixture formed by the bromination of 1-aminoanthraquinone-2-sulphonic acid in sulphuric acid, which process comprises adjusting the sulphuric acid concentration of the reaction mixture under the prevailing conditions of temperature and pressure to effect precipitation of 1-amino-4-bromoanthraquinone-2-sulphonic acid as the sulphate and thereafter separating the resultant sulphate precipitate from the reaction mixture.
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- Process for the preparation of 1-amino-4-bromoanthraquinone-2-sulphonic acid I
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A process for preparing 1-amino-4-bromoanthraquinone-2-sulphonic acid or an alkali metal salt thereof which comprises contacting 1-amino-anthraquinone at a temperature in the range of 90° to 150° C. with an SO3 -containing sulphuric acid (oleum) and thereafter treating the resultant sulphonated 1-amino-anthraquinone with at least 0.5 molar equivalent of bromine, relative to 1 mol of 1-amino-anthraquinone, at temperatures in the range from 60° to 100° C.
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