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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 three wastes in the reduction process, and does not fundamentally change the disadvantages of the process.
With increasingly stringent environmental protection requirements, traditional production methods have no prospects for development

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

Embodiment 1

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

[0019]

[0020] Add 94 grams of aniline, 100 grams of concentrated sulfuric acid (concentrated sulfuric acid with a concentration of 98%), and 120 grams of sodium bisulfate into the disperser in turn, disperse for 1 hour, then pour the uniformly dispersed material into a baking tray, and put it into a vacuum drying In the box, heat to 200°C, keep warm for 18 hours, pour the material into 600ml of water, add 1 gram of activated carbon, heat to 80°C for decolorization, filter out the activated carbon after decolorization, stir, cool to room temperature, crystallize, filter to obtain white Solid 168 grams, content: 99%. The filtrate was applied to the next batch.

Embodiment 2

[0022] Synthesis of anthranilic acid

[0023] Add 94 grams of aniline, 100 grams of concentrated sulfuric acid, and 136 grams of potassium bisulfate into the disperser in sequence, and disperse for 1 hour, then pour the uniformly dispersed materials into a baking tray, put them in a vacuum drying oven, heat to 210°C, and keep warm After 18 hours, the material was poured into the water (600ml) obtained in Example 1, and 1 gram of activated carbon was added, heated to 80°C for decolorization, and the activated carbon was filtered after decolorization, stirred, crystallized, and filtered to obtain 170 grams of white solid, content : 99%. The filtrate was applied to the next batch.

Embodiment 3

[0025] Synthesis of anthranilic acid

[0026] Add 94 grams of aniline, 100 grams of concentrated sulfuric acid, and 144 grams of sodium bisulfate into the disperser in sequence, and disperse for 1 hour, then pour the uniformly dispersed materials into a baking tray, put them in a vacuum drying oven, heat to 210°C, and keep warm After 18 hours, the material was poured into the water (600ml) obtained in Example 2, and 1 gram of activated carbon was added, heated to 80° C. for decolorization, and the activated carbon was filtered after decolorization, stirred, crystallized, and filtered to obtain 172 grams of white solid, content : 99%. The filtrate is evaporated to recover 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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