Preparation method of para-(beta-Ethyl Sulfonyl Sulfate) aniline sulfonic acid

Abstract

The present invention is a kind of preparation method of p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid, it is characterized in that: adopt concentrated sulfuric acid (100%) as solvent, p-(β-sulfate ethyl sulfone) aniline As a raw material, it is dispersed at a temperature of 60-90°C, sulfonated at 120-130°C, hydrolyzed at 100-110°C, cooled, acidified, crystallized, filtered, and dried to obtain the product. With the p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid prepared by the inventive method, the reactive dyes made by it are compared with the reactive dyes made from p-(β-sulfate ethyl sulfone) aniline, Its dyeing depth, color fixing rate, solubility, salt and alkali resistance stability, and wet rubbing fastness are all improved, and the washability is better.

Description

technical field

[0001] The invention relates to a preparation method of intermediates of three primary colors of dyes, in particular to a preparation method of p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid. Background technique

[0002] As we all know, p-(β-sulfate ethyl sulfone) aniline is one of the important intermediates for the preparation of the three primary colors of reactive dyes, but the performance of the dyes synthesized by it needs to be further improved. Contents of the invention

[0003] The purpose of this invention is to provide a kind of preparation method of p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid, the p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid prepared by the inventive method, by Compared with the reactive dyes prepared with p-(β-sulfate ethyl sulfone) aniline, the reactive dyes produced by it have better dyeing depth, color fixation rate, solubility, salt and alkali resistance stability, and wet rubbing fastness. It has been...

Examples

Embodiment 1

[0021] Embodiment 1: Use concentrated sulfuric acid, p-(β-sulfate ethyl sulfone) aniline to add dilute hydrochloric acid to prepare intermediate p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid, the steps are as follows:

[0022] 1. Disperse, add 1000kg of concentrated sulfuric acid (100%) into the reaction pot, slowly add 696kg of p-(β-sulfate ethyl sulfone) aniline (100%) under constant stirring, control the temperature at 80-85°C, beat After 2 hours, check the dispersion of p-(β-sulfate ethyl sulfone) aniline to make it exist without lumps;

[0023] 2. Sulfonation, turn on the steam and slowly heat up to 125-130°C, and react at this temperature for 8 hours, and detect by high performance liquid chromatography (HPLC), if p-(β-sulfate ethyl sulfone) aniline≤0.5% , then the sulfonation is in place, such as p-(β-sulfate ethyl sulfone) aniline>0.5%, then continue the insulation reaction until p-(β-sulfate ethyl sulfone) aniline≤0.5%.

[0024] 3. Hydrolysis, after cooling the...

Embodiment 2

[0026] Embodiment 2: Use concentrated sulfuric acid, p-(β-sulfate ethyl sulfone) aniline to add dilute sulfuric acid to prepare intermediate p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid, the steps are as follows:

[0027] 1. Disperse, add 1000kg of concentrated sulfuric acid (100%) into the reaction pot, slowly add 696kg of p-(β-sulfate ethyl sulfone) aniline (100%) under constant stirring, control the temperature at 80-85°C, beat After 2 hours, check the dispersion of p-(β-sulfate ethyl sulfone) aniline, if there is no block, proceed to the next step;

[0028] 2. Turn on the steam and slowly heat up to 125-130°C, and react at this temperature for 8 hours, detect with high performance liquid chromatography (HPLC), if p-(β-sulfate ethyl sulfone) aniline≤0.5%, then The sulfonation is in place; if p-(β-sulfate ethylsulfone) aniline>0.5%, the heat preservation reaction should be continued until p-(β-sulfate ethylsulfone)aniline≤0.5% is qualified;

[0029] 3. After cooling ...

technical field

[0001] The invention relates to a preparation method of intermediates of three primary colors of dyes, in particular to a preparation method of p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid. Background technique

[0002] As we all know, p-(β-sulfate ethyl sulfone) aniline is one of the important intermediates for the preparation of the three primary colors of reactive dyes, but the performance of the dyes synthesized by it needs to be further improved. Contents of the invention

[0003] The purpose of this invention is to provide a kind of preparation method of p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid, the p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid prepared by the inventive method, by Compared with the reactive dyes prepared with p-(β-sulfate ethyl sulfone) aniline, the reactive dyes produced by it have better dyeing depth, color fixation rate, solubility, salt and alkali resistance stability, and wet rubbing fastness. It has been...

Examples

Embodiment 1

[0021] Embodiment 1: Use concentrated sulfuric acid, p-(β-sulfate ethyl sulfone) aniline to add dilute hydrochloric acid to prepare intermediate p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid, the steps are as follows:

[0022] 1. Disperse, add 1000kg of concentrated sulfuric acid (100%) into the reaction pot, slowly add 696kg of p-(β-sulfate ethyl sulfone) aniline (100%) under constant stirring, control the temperature at 80-85°C, beat After 2 hours, check the dispersion of p-(β-sulfate ethyl sulfone) aniline to make it exist without lumps;

[0023] 2. Sulfonation, turn on the steam and slowly heat up to 125-130°C, and react at this temperature for 8 hours, and detect by high performance liquid chromatography (HPLC), if p-(β-sulfate ethyl sulfone) aniline≤0.5% , then the sulfonation is in place, such as p-(β-sulfate ethyl sulfone) aniline>0.5%, then continue the insulation reaction until p-(β-sulfate ethyl sulfone) aniline≤0.5%.

[0024] 3. Hydrolysis, after cooling the...

Embodiment 2

[0026] Embodiment 2: Use concentrated sulfuric acid, p-(β-sulfate ethyl sulfone) aniline to add dilute sulfuric acid to prepare intermediate p-(β-sulfate ethyl sulfone) aniline o-sulfonic acid, the steps are as follows:

[0027] 1. Disperse, add 1000kg of concentrated sulfuric acid (100%) into the reaction pot, slowly add 696kg of p-(β-sulfate ethyl sulfone) aniline (100%) under constant stirring, control the temperature at 80-85°C, beat After 2 hours, check the dispersion of p-(β-sulfate ethyl sulfone) aniline, if there is no block, proceed to the next step;

[0028] 2. Turn on the steam and slowly heat up to 125-130°C, and react at this temperature for 8 hours, detect with high performance liquid chromatography (HPLC), if p-(β-sulfate ethyl sulfone) aniline≤0.5%, then The sulfonation is in place; if p-(β-sulfate ethylsulfone) aniline>0.5%, the heat preservation reaction should be continued until p-(β-sulfate ethylsulfone)aniline≤0.5% is qualified;

[0029] 3. After cooling ...

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