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Preparation method of para-(beta-Ethyl Sulfonyl Sulfate) aniline sulfonic acid
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A kind of technology of sulfate ethyl sulfone and aniline ortho, applied in the field of preparation of intermediates
Inactive Publication Date: 2007-09-19
HUBEI HUALI DYESTUFF INDAL
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[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
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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 heat preservation reaction until p-(β-sulfate ethyl sulfone) aniline ≤ 0.5%.
[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 Sulfonated in place; if p-(β-sulfate ethylsulfone) aniline > 0.5%, continue the heat preservation reaction until p-(β-sulfate ethylsulfone) aniline ≤ 0.5% is qualified;
[0029] 3. After cooling the sulfonated...
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Abstract
The invention is a producing method of a p-(beta-sulfooxyethylsulfone)phenylamine-o-sulfonic acid, which is characterized in that: having the oil of vitriol (100%) as solvent, p-(beta-sulfooxyethylsulfone)phenylamine as material, dispersing at about 60-90 DEG C, sulfonating at 120-130 DEG C, hydrolyze at 100-110 DEG C, then cooling, acidifying, crystallizing, filtering, drying to get product. The active dye produced by p-(beta-sulfooxyethylsulfone)phenylamine-o-sulfonic acid has a better pile-on property, fixing rate, solubility, alkaline saline resistance, humidity resistance, friction fastness compared the dye produced by p-(beta-sulfooxyethylsulfone)phenylamine.
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. There is im...
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