Preparation process of bromamine acid

A preparation process and a technology for bromoamino acid, applied in the field of organic synthesis, can solve the problems of reducing yield, reaction temperature, side reactions, by-products, etc., and achieve the effects of reasonable parameter design, reduction of side reactions, and cost saving.

Inactive Publication Date: 2017-05-31
TAIZHOU DONGFENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 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 reduction reaction The mixture, because the reaction of generating 1-nitroanthraquinone is an exothermic reaction, the exothermic reaction is easy to cause the reaction temperature to be too high to cause the occurrence of side reactions, resulting in a large number of by-products, and the generation of by-products affects the purity of the product , while reducing the yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Step 1: Nitrification reaction, add 5000kg of dichloroethane, 1260kg of anthraquinone, and 375kg of nitric acid into the reaction kettle, then slowly and evenly drop the amount of mixed acid to be 197kg, and the reaction will generate 1-nitroanthraquinone;

[0042] Step 2: The product in step 1 is diluted with water, crystallized and filtered to obtain a dry product;

[0043] Step 3: Reduction reaction, at normal temperature, add 1000kg of water to the reaction kettle, then add the dry product 1-nitroanthraquinone in step 2 to the reaction kettle, stir and mix evenly to be muddy, then add 1830kg of sodium sulfate aqueous solution, Heating to 80°C for reduction reaction to produce 1-aminoanthraquinone;

[0044] Step 4: Sulfonation reaction, add 9000kg of o-dichlorobenzene in the sulfonation kettle, heat, then add the crude product 1-aminoanthraquinone in step 3, slowly add 470kg of chlorosulfonic acid at a negative pressure of 200mmHg and a temperature of 80°C Reaction,...

Embodiment 2

[0049] Step 1: Nitrification reaction, add 5000kg of dichloroethane, 1260kg of anthraquinone, 425kg of nitric acid in the reaction kettle, then slowly and evenly drop the amount of sulfuric acid to be 276kg, and the reaction will generate 1-nitroanthraquinone;

[0050] Step 2: The product in step 1 is diluted with water, crystallized and filtered to obtain a dry product;

[0051]Step 3: Reduction reaction, at normal temperature, add 1000kg of water to the reaction kettle, then add the dry product 1-nitroanthraquinone in step 2 to the reaction kettle, stir and mix evenly to be muddy, then add 1887kg of sodium sulfate aqueous solution, Heating to 90°C for reduction reaction to produce 1-aminoanthraquinone;

[0052] Step 4: Sulfonation reaction, add 9000kg of o-dichlorobenzene into the sulfonation kettle, then add the crude product 1-aminoanthraquinone in step 3, heat, and slowly add 610kg of chlorosulfonic acid at a negative pressure of 200mmHg and a temperature of 80°C Reactio...

Embodiment 3

[0057] Step 1: Nitrification reaction, add 5000kg of dichloroethane, 1260kg of anthraquinone, 500kg of nitric acid in the reactor, then slowly and evenly drop the amount of sulfuric acid to be 395kg, and the reaction will generate 1-nitroanthraquinone;

[0058] Step 2: The product in step 1 is diluted with water, crystallized and filtered to obtain a dry product;

[0059] Step 3: reduction reaction, at normal temperature, add 1000kg of water to the reaction kettle, then add the dry product 1-nitroanthraquinone in step 2 to the reaction kettle, stir and mix evenly to be muddy, then add 1944kg of sodium sulfate aqueous solution, Heating to 100°C for reduction reaction to produce 1-aminoanthraquinone;

[0060] Step 4: Sulfonation reaction, add 9000kg of o-dichlorobenzene into the sulfonation kettle, then add the crude product 1-aminoanthraquinone in step 3, heat, and slowly add 657kg of chlorosulfonic acid at a negative pressure of 200mmHg and a temperature of 80°C Reaction, the...

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Abstract

The invention discloses a preparation process of bromamine acid. The preparation process is characterized by comprising the following steps of carrying out nitration reaction, reduction reaction, sulfonation reaction and bromination reaction and finally refining to prepare the bromamine acid from anthraquinone; reaction conditions and a process step of adding materials are reasonably designed, so that the generated bromamine acid has high purity and the yield is relatively high.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation process of 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. [0004] 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 r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/53C07C303/22
CPCC07C303/22C07C201/08C07C221/00C07C303/08
Inventor 王海波
Owner TAIZHOU DONGFENG CHEM CO LTD
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