Method for preparing aniline-2-sulfonic acid

A technology for o-aminobenzenesulfonic acid and aniline, which is applied in the field of preparing o-aminobenzenesulfonic acid by catalytic sulfonation of aniline, can solve the problems of no development prospect, large three wastes, low yield and the like, and achieves low cost, less three wastes, and a process route. short effect

Active Publication Date: 2016-04-13
SHENYANG RES INST OF CHEM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The disadvantages of the above process are long route, large amount of three wastes, and low yield. Although the nitro hydrogenation reduction process replaces the iron powder reduction process, it can only reduce part of the th

Method used

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  • Method for preparing aniline-2-sulfonic acid
  • Method for preparing aniline-2-sulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0017] Example 1

[0018] The synthesis of anthranilic acid, the reaction formula is as follows:

[0019]

[0020] Add 94 grams of aniline, 100 grams of concentrated sulfuric acid (98% concentrated sulfuric acid), and 120 grams of sodium bisulfate to the disperser, and disperse for 1 hour, then pour the uniformly dispersed materials into the baking tray and put them in vacuum to dry In the box, heat to 200℃ and keep for 18 hours, pour the material into 600ml water, add 1g activated carbon, heat to 80℃ to decolorize, filter out the activated carbon after decolorization, stir, cool to room temperature, crystallize, filter, and get white Solid 168 grams, content: 99%. The filtrate is applied to the next batch.

Example Embodiment

[0021] Example 2

[0022] Synthesis of anthranilic acid

[0023] Add 94 grams of aniline, 100 grams of concentrated sulfuric acid, and 136 grams of potassium hydrogen sulfate to the disperser in turn, and disperse for 1 hour, then pour the uniformly dispersed materials into a baking pan, put them in a vacuum drying oven, and heat to 210°C and keep warm After 18 hours, pour the material into the water (600ml) obtained in Example 1, and add 1g of activated carbon, heat to 80°C for decolorization, filter out the activated carbon after decolorization, stir, crystallize, and filter to obtain 170 grams of white solid. : 99%. The filtrate is applied to the next batch.

Example Embodiment

[0024] Example 3

[0025] Synthesis of anthranilic acid

[0026] Add 94 grams of aniline, 100 grams of concentrated sulfuric acid, and 144 grams of sodium bisulfate to the disperser in turn, and disperse for 1 hour, then pour the uniformly dispersed materials into a baking pan, put them in a vacuum drying oven, and heat to 210°C and keep warm. After 18 hours, pour the material into the water (600ml) obtained in Example 2, and add 1 g of activated carbon, heat to 80°C for decolorization, filter out the activated carbon after decolorization, stir, crystallize, and filter to obtain 172 grams of white solid. : 99%. The filtrate evaporates water and recovers sodium bisulfate.

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Abstract

The invention relates to a method for preparing aniline-2-sulfonic acid, in particular to a method for preparing aniline-2-sulfonic acid through aniline catalysis and sulfonation. With metal hydrogen sulfate serving as a catalyst, aniline is directly catalyzed and sulfonated to prepare aniline-2-sulfonic acid in a transposition mode. According to the method, aniline is directly catalyzed and sulfonated to prepare aniline-2-sulfonic acid in the transposition mode, so that aniline-2-sulfonic acid is prepared from aniline through a one-step method, and the total yield of aniline-2-sulfonic acid reaches 95% or above; the process route is short, the quantity of the three wastes is small, and the cost is low.

Description

technical field [0001] The invention relates to a method for preparing anthranilic acid, in particular to a method for preparing anthranilic acid by catalytic sulfonation of aniline. Background technique [0002] Anthranilic acid is an important chemical intermediate, which is widely used in the production of dyes, pesticides, medicines and other fields. Since aniline and sulfuric acid are salted and translocated to generate p-aminobenzenesulfonic acid, the current domestic preparation method is o-chloronitrobenzene and Sodium disulfide is co-heated in alcohol to convert it into 2,2-dinitrodiphenyl disulfide, then oxidize it with chlorine gas into o-nitrobenzenesulfonyl chloride, hydrolyze it into o-nitrobenzenesulfonic acid with sodium carbonate, and then use iron powder or hydrogenation reduction of nitro into amino groups to obtain o-aminobenzenesulfonic acid, CN101362710, CN1066446, Chemical Production and Technology (2009), 16(4), 23-24. Sulfonated to generate o-nitrob...

Claims

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Application Information

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IPC IPC(8): C07C309/46C07C303/06
CPCC07C303/06C07C309/46
Inventor 闫士杰李付刚李文骁
Owner SHENYANG RES INST OF CHEM IND
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