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Preparation method for bromamine acid

A technology of bromic acid and sodium sulfate, which is applied in the field of medicine and chemical industry, can solve the problems of unsuitability for industrial production, harsh reaction conditions, complicated process flow, etc., and achieve the effects of low production cost, mild reaction conditions and high total reaction yield

Inactive Publication Date: 2019-05-10
MAANSHAN DEHONG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] CN201611041314 reported that anthraquinone was used as raw material to obtain bromonic acid through nitration reaction, reduction reaction, sulfonation and bromination reaction, and refined. The process of this method is complicated, the reaction conditions are harsh, and it is not suitable for industrial production

Method used

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  • Preparation method for bromamine acid
  • Preparation method for bromamine acid
  • Preparation method for bromamine acid

Examples

Experimental program
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Effect test

Embodiment 1

[0037] A preparation method for bromic acid, comprising the following steps:

[0038] Add 200ml of 20% oleum and 100g of anhydrous sodium sulfate into a three-necked flask with stirring, start stirring, weigh 150g of 1-aminoanthraquinone, and 750g of o-dichlorobenzene, slowly add them to the three-necked flask, heat up to 150°C and keep warm 3h; Cool the reaction solution to 80°C, add 0.2g of iodine and 0.5ml of anti-foaming agent, and slowly add 21ml of bromine dropwise within 6h, keep the temperature for 2h after dripping; remove excess bromine by distillation under reduced pressure, add 150ml of bromine to the reaction solution Water, cooled to 50°C, suction filtered to obtain 668g of filter cake; add the filter cake to 1500ml water and heat up to 90°C, and add 50% sodium hydroxide solution to adjust pH = 8, cool to 30°C, and suction filter to obtain the product bromine 238.4g, the yield is 92%, and the purity detected by liquid chromatography is 99%.

Embodiment 2

[0040] A preparation method for bromic acid, comprising the following steps:

[0041] Add 200ml of 20% oleum and 100g of anhydrous sodium sulfate into a three-necked flask with stirring, start stirring, weigh 150g of 1-aminoanthraquinone and 750g of o-dichlorobenzene and slowly add them into the three-necked flask, heat up to 100°C and keep warm 10h; cool the reaction solution to 80°C, add 0.2g of iodine and 0.5ml of anti-foaming agent, and slowly add 21ml of bromine dropwise within 6h, and keep warm for 2h after dropping; remove excess bromine by distillation under reduced pressure, and add 150ml of bromine to the reaction solution Water, cooled to 50°C, suction filtered to obtain 668g of filter cake; add the filter cake to 1500ml water and heat up to 90°C, and add 50% sodium hydroxide solution to adjust pH = 8, cool to 30°C, and suction filter to obtain the product bromine 238.4g, the yield is 92%, and the purity detected by liquid chromatography is 99%.

Embodiment 3

[0043] A preparation method for bromic acid, comprising the following steps:

[0044] Add 200ml of 20% oleum and 100g of anhydrous sodium sulfate into a three-necked flask with stirring, start stirring, weigh 150g of 1-aminoanthraquinone, and 750g of o-dichlorobenzene, slowly add them into the three-necked flask, heat up to 130°C and keep warm 5h; cool the reaction solution to 80°C, add 0.2g of iodine and 0.5ml of anti-foaming agent, and slowly add 21ml of bromine dropwise within 5h. Water, cooled to 50°C, suction filtered to obtain 668g of filter cake; add the filter cake to 1500ml water and heat up to 90°C, and add 50% sodium hydroxide solution to adjust pH = 8, cool to 30°C, and suction filter to obtain the product bromine 238.4g, the yield is 92%, and the purity detected by liquid chromatography is 99%.

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Abstract

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%.

Description

technical field [0001] The invention relates to the technical field of medicine and chemical industry, in particular to a preparation method of bromic acid. Background technique [0002] Bromonic acid, the chemical name is 1-amino-4-bromo-2-sulfonic acid anthraquinone, which is a dye intermediate used in the preparation of acid anthraquinone dyes, such as weak acid brilliant blue R and reactive brilliant blue M -BR and Brilliant Blue KGR etc. [0003] The existing production method of bromic acid is to use 1-aminoanthraquinone as raw material, drip chlorosulfonic acid in o-dichlorobenzene solvent to carry out sulfonation reaction, after the sulfonation reaction reaches the end point, first distill and reclaim o-dichlorosulfonic acid Benzene, then add water to the reaction system, dilute the sulfonated material to the acidity required for the bromination reaction (the mass percent concentration of sulfuric acid in the sulfonated material is 8% to 10%), and then add bromine d...

Claims

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Application Information

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IPC IPC(8): C07C303/22C07C309/53
Inventor 祁超杨建平魏慧龙沈梦桐
Owner MAANSHAN DEHONG BIOTECH
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