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Production method of 6-nitro-1,2,4-sulfonic acid

A production method and technology of acid oxides, applied in the direction of organic chemistry, etc., can solve the problems of difficult treatment and high production cost of waste gas, and achieve the effects of reducing dosage, improving quality and improving solubility

Active Publication Date: 2014-05-07
JIANGSU YUANZHENG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is to provide a new production method of 6-nitro-1,2,4-acid oxygen body to solve the problem of producing a large amount of difficult-to-handle high COD in the production process. Problems of waste water, waste gas and high production cost

Method used

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  • Production method of 6-nitro-1,2,4-sulfonic acid

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Effect test

Embodiment 1

[0031] Embodiment 1, a kind of production method of 6-nitro-1,2,4-acid oxygen body, its steps are as follows:

[0032] (1) Use ethyl naphthol as raw material, add bottom water, slowly heat up to 50°C until ethyl naphthol dissolves, beat at 50°C and keep warm for 20 minutes, then cool down to 20°C; the bottom water and ethyl naphthol The weight ratio of phenol is 0.8: 1.0; Described bottom water is water;

[0033] (2) Nitrosation: Add solid sodium nitrite, beat for 20 minutes, cool down to 0°C, start adding the prepared sulfuric acid solution dropwise, and control the dropping time to 3 hours. Slowly add liquid caustic soda at 10°C to make the system pH to 4; the weight ratio of sodium nitrite, sulfuric acid, ethyl naphthol=0.45:0.34:1.0, the concentration of sulfuric acid solution is 5%;

[0034] (3) Sulfonation and reductive translocation: add sodium metabisulfite, keep warm for 20 minutes, then raise the temperature to 15°C, keep warm for 0.5 hours, stop stirring, stand sti...

Embodiment 2

[0037] Embodiment 2, a kind of production method of 6-nitro-1,2,4-acid oxygen body, its steps are as follows:

[0038] (1) Use ethyl naphthol as raw material, add bottom water, slowly heat up to 80°C until ethyl naphthol dissolves, beat at 80°C and keep warm for 40 minutes, then cool down to 40°C; the bottom water and ethyl naphthol The weight ratio of phenol is 1.5:1.0; the bottom water is water, the reaction mother liquor (the filtrate produced by filtering in step (3), or the mother liquor and filtrate produced by the washing in step (4)) or a mixture of the two;

[0039] (2) Nitrosation: Add solid sodium nitrite, beat for 40 minutes, cool down to 10°C, start adding the prepared sulfuric acid solution dropwise, and control the dropping time to 8 hours. Slowly add liquid caustic soda at 20°C to make the system pH to 7; the weight ratio of sodium nitrite, sulfuric acid and ethyl naphthol=0.55:0.68:1.0, the concentration of sulfuric acid solution is 30%;

[0040](3) Sulfonati...

Embodiment 3

[0043] Embodiment 3, a kind of production method of 6-nitro-1,2,4-acid oxygen body, its steps are as follows: add 800 parts of bottom water (both parts by weight, the same below) in the reactor, drop in ethyl naphthalene 1000 parts of phenol, slowly heat up to 50°C, observe whether ethyl naphthol is dissolved, beat at 50°C and keep warm for half an hour, then cool down to 20°C, add 450 parts of solid sodium nitrite, beat for half an hour, cool to 0°C, Start to drop 340 parts (100 percent) of the configured sulfuric acid solution, the solubility of the sulfuric acid solution is 30%, the dropping time is controlled to 3 hours, the dropping is completed, and the heat preservation reaction is 1 hour. Then raise the temperature to 10°C and slowly add liquid caustic soda to make the system pH to 4. Then add 1500 parts of sodium metabisulfite, keep the reaction for 0.5 hours, then raise the temperature to 15° C., keep the reaction for 1 hour, stop stirring, stand still, and filter. ...

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Abstract

The invention relates to a production method of a dye intermediate, i.e., 6-nitro-1,2,4-sulfonic acid. The method is characterized in that: the 6-nitro-1,2,4-sulfonic acid is obtained by taking ethyl naphthol as a major raw material and performing procedures including nitrosification, neutralizing, sulfonation reduction displacement, diazotization, acidification, nitration and the like. Due to the adoption of the method, the problems of the production of a large amount of high-COD (Chemical Oxygen Demand) waste water and waste gas and high production cost existing in a production process can be solved. In the method, ethyl naphthol is dissolved by raising the temperature naturally, so that a liquid caustic soda dissolving method is replaced, the using amount of liquid caustic soda and sulfuric acid is reduced, production cost is reduced, and the production of waste water is reduced; a diazonium resisting method is adopted for diazonium, so that the production of toxic waste gas is reduced, the yield of diazonium is increased, and production cost is reduced; the diazonium resisting method is adopted, and solid sodium nitrite is added, so that the production of waste water can be reduced; and in diazonium, copper sulfate is taken as a catalyst, so that reaction speed is increased, the occurrence of side reactions is reduced, and yield is increased.

Description

technical field [0001] The invention relates to a production method of a dye intermediate, in particular to a production method of 6-nitro-1,2,4-acid oxygen body. Background technique [0002] 6-nitro-1,2-diazooxynaphthalene-4-sulfonic acid, also known as 6-nitro-1,2,4-acid oxygen body, 6-nitro body. This is an important dye intermediate, widely used in the synthesis of acid and acid mordant dyes, such as media black T, acid black 172.194, etc. [0003] In the traditional process of nitrosation process, liquid caustic soda is used to dissolve ethyl naphthol first, then acidified, and sodium nitrite is added dropwise to carry out nitrosation. Salt wastewater. 1.2.4-Acid diazotization process, adopt positive diazonium method (add acid to filter cake, then add sodium nitrite dropwise), quickly add sodium nitrite dropwise, produce a lot of yellow smoke, and the yield is low. The reaction formula is as follows: [0004] Nitrosation: [0005] [0006] Diazotization: [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D271/12
Inventor 程燕明王海民叶丽丽韩军杨洋
Owner JIANGSU YUANZHENG CHEM
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