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Preparation method of bromoamine acid

A technology of bromic acid and dilute sulfuric acid, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of many side reactions, high energy consumption, and many impurities in sulfonated materials, so as to improve the purity, improve the quality, and reduce energy consumption Effect

Active Publication Date: 2012-08-01
苏州市罗森助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is that the solvent ortho-dichlorobenzene must be recovered every time, the energy consumption is large, the process is cumbersome, and the impurities in the sulfonated material are more, so that there are more side reactions during bromination, so the purity of the product bromonic acid is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation method of the bromic acid of the present embodiment comprises the steps:

[0015] (1) Sulfonation reaction: Add 1800kg of o-dichlorobenzene into the sulfonation kettle, heat it, then add 300kg of 1-aminoanthraquinone, cover the pot tightly, raise the temperature to 85°C under a negative pressure of 500mmHg, and dehydrate for 2 hours. After completion, slowly add 247kg of chlorosulfonic acid dropwise under the condition of vacuum degree of 200mmHg, continue to stir for 1 hour after the addition, then raise the temperature to 125-130°C and keep for 5 hours, take samples, and measure the end point.

[0016] (2) Layering with dilute sulfuric acid: After the end point of the sulfonation reaction is reached, add 500kg of dilute sulfuric acid with a concentration of 55wt% into the sulfonation kettle to make the acidity of the sulfonated material 60%~65%, and the sulfonated material is layered. The upper layer is the organic phase of o-dichlorobenzene, and...

Embodiment 2

[0020] The preparation method of the bromic acid of the present embodiment comprises the steps:

[0021] (1) Sulfonation reaction: Add 1500kg of o-dichlorobenzene into the sulfonation kettle, heat it, then add 300kg of 1-aminoanthraquinone, cover the pot tightly, raise the temperature to 85°C under a negative pressure of 500mmHg, and dehydrate for 2 hours. After completion, slowly add 247kg of chlorosulfonic acid dropwise under the condition of vacuum degree of 200mmHg, continue to stir for 1 hour after the addition, then raise the temperature to 125-130°C and keep for 5 hours, take samples, and measure the end point.

[0022] (2) Layering with dilute sulfuric acid: After the end point of the sulfonation reaction is reached, add 460kg of dilute sulfuric acid with a concentration of 60wt% into the sulfonation kettle to make the acidity of the sulfonated material about 60%~65%, and the sulfonated material is layered , the upper layer is the organic phase of o-dichlorobenze...

Embodiment 3

[0026] The preparation method of the bromic acid of the present embodiment comprises the steps:

[0027] (1) Sulfonation reaction: Add 2100kg o-dichlorobenzene into the sulfonation kettle, heat it, then add 300kg 1-aminoanthraquinone, cover the pot tightly, raise the temperature to 85°C under a negative pressure of 500mmHg, and dehydrate for 2 hours. After completion, slowly add 247kg of chlorosulfonic acid dropwise under the condition of vacuum degree of 200mmHg, continue to stir for 1 hour after the addition, then raise the temperature to 125-130°C and keep for 5 hours, take samples, and measure the end point.

[0028] (2) Layering with dilute sulfuric acid: After the end point of the sulfonation reaction is reached, add 500kg of dilute sulfuric acid with a concentration of 55wt% into the sulfonation kettle to make the acidity of the sulfonated material 60%~65%, and the sulfonated material is layered. The upper layer is the organic phase of o-dichlorobenzene, and the l...

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PUM

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Abstract

The invention relates to a preparation method of bromoamine acid, which comprises the following steps: (1) sulfonation reaction: by using 1-aminoanthraquinone as a raw material, dropwisely adding chlorosulfonic acid into an orthodichlorobenzene solvent to carry out sulfonation reaction so as to obtain the sulfonated material containing sulfonated product, wherein the weight ratio of the 1-aminoanthraquinone to the orthodichlorobenzene is 1:(5-7), and the temperature of the sulfonation reaction is 115-150 DEG C; (2) stratification by adding dilute sulfuric acid: after the sulfonation reaction reaches to the end, directly adding 55-60 wt% dilute sulfuric acid into the reaction system until the sulfonated material stratifies, wherein the upper stratum is an orthodichlorobenzene organic phase which can be used repeatedly, and the understratum is a sulfuric acid solution of 1-aminoanthraquinone-2-sulfonic acid; and (3) bromination reaction: adding water into the understratum material obtained in the step (2) until the acidity reaches to 8-10%, and directly dropwisely adding bromine to carry out bromination reaction, thereby obtaining the bromoamine acid crude product. The invention greatly lowers the energy consumption; and the quality and yield of the bromoamine acid product are obviously enhanced.

Description

technical field [0001] The invention relates to a preparation method 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] 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 percentage concentration of sulfuric acid in the sulfonated material is 8%~10%), and then a...

Claims

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Application Information

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IPC IPC(8): C07C309/53C07C303/22
Inventor 李根荣徐新连
Owner 苏州市罗森助剂有限公司
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